CN105777974A - Preparation method of temperature-sensitive magnetic high-hygroscopicity resin for fine mineral dewatering - Google Patents

Preparation method of temperature-sensitive magnetic high-hygroscopicity resin for fine mineral dewatering Download PDF

Info

Publication number
CN105777974A
CN105777974A CN201610163954.3A CN201610163954A CN105777974A CN 105777974 A CN105777974 A CN 105777974A CN 201610163954 A CN201610163954 A CN 201610163954A CN 105777974 A CN105777974 A CN 105777974A
Authority
CN
China
Prior art keywords
temperature sensitive
preparation
fine mineral
paa
mass ratio
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201610163954.3A
Other languages
Chinese (zh)
Other versions
CN105777974B (en
Inventor
张素红
杨志超
刘生玉
郭建英
乔燕
陈航超
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Taiyuan University of Technology
Original Assignee
Taiyuan University of Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Taiyuan University of Technology filed Critical Taiyuan University of Technology
Priority to CN201610163954.3A priority Critical patent/CN105777974B/en
Publication of CN105777974A publication Critical patent/CN105777974A/en
Application granted granted Critical
Publication of CN105777974B publication Critical patent/CN105777974B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • 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
    • C08F220/04Acids; Metal salts or ammonium salts thereof
    • C08F220/06Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
    • CCHEMISTRY; METALLURGY
    • 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
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/24Crosslinking, e.g. vulcanising, of macromolecules
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • CCHEMISTRY; METALLURGY
    • 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
    • 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
    • C08J2333/02Homopolymers or copolymers of acids; Metal or ammonium salts thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2265Oxides; Hydroxides of metals of iron
    • C08K2003/2275Ferroso-ferric oxide (Fe3O4)

Abstract

The invention discloses a preparation method of temperature-sensitive magnetic high-hygroscopicity resin for fine mineral dewatering and belongs to the technical field of functional materials and solid-liquid separation. The preparation method of a composite material includes: using raw materials FeSO4-7H2O and Fe(NO3)3-9H2O to form a colloidal solution; adding sodium acrylate, acrylic acid, temperature-sensitive monomer, a cross-linking agent and an initiator. The temperature-sensitive magnetic high-hygroscopicity resin synthesized has lowest critical solution temperature (LCST), and water in the resin after absorbing water is discharged for regeneration in a non-phase-change manner. By using the preparation method, the high-hygroscopicity resin with stable temperature-sensitive magnetism and a composite structure can be prepared quickly and can be used for dewatering fine mineral materials.

Description

A kind of fine mineral is dehydrated the preparation method of temperature sensitive magnetic high hydroscopic resin
Technical field
The invention belongs to functional material and solid-liquid separation technique field, relate to the preparation method of a kind of temperature sensitive magnetic high hydroscopic resin for fine mineral dehydration, the method can quickly prepare the high hydroscopic resin with the composite construction stablizing temperature sensitive magnetic.
Background technology
Temperature sensitive magnetic high hydroscopic resin is a kind of to have the functional high molecule material that high-hydroscopicity, Thermo-sensitive and three kinds of characteristics of magnetic are integrated concurrently.Chinese patent CN103172958A discloses a kind of Thermo-sensitive epoxy resin composite material and preparation method thereof, and it is mainly used in the field such as smart coatings and functional plastics.Chinese patent CN104072693A discloses the preparation method of a kind of temperature sensing polymer grafting carbon ball compound, and main purpose is the range of application expanding material with carbon element carbon ball.Additionally Chinese patent CN103657546A discloses a kind of method preparing core-shell structure magnetic compound resin microballoon, first magnetic ferroferric oxide nano-particles is prepared, then under the conditions of microwave hydrothermal, with ferriferrous oxide nano-particle as seed, phenol and formaldehyde are coated to the surface of ferroso-ferric oxide by in-situ polymerization.Above patent adds solid magnetic material grains during synthesizing magnetic macromolecular material and is difficult to avoid the shortcomings such as magnetic homogeneity is poor, magnetic content is low, magnetic is more weak, and the resin being provided simultaneously with high-hydroscopicity, Thermo-sensitive and three kinds of good characteristics of magnetic is particularly difficult.
Fine mineral dehydration at present is a big technical barrier of mineral processing and utilization industry, use super absorbent resin fine mineral is dehydrated be a kind of brand-new by means of absorbent material to remove the method for moisture in fine mineral, but moisture in super absorbent resin removing fine mineral, its dehydration is easily controlled, and after absorbing water, recovery and the regeneration of resin are highly difficult.Therefore synthesize temperature sensitive magnetic high hydroscopic resin and be applied to fine mineral dehydration, by magnetic separation separation resin, recycling with non-phase transformation dehydration regeneration by Thermo-sensitive afterwards, thus saved big energy, also it is the breakthrough solving a fine mineral dehydration technique difficult problem, is theoretical extension and the technology application realizing fine mineral dehydration.
Summary of the invention
During for water-absorbing resin difference prepared by existing method, there is temperature sensitive, magnetic and high-hydroscopicity is integrated, and there is the technical problem that magnetic homogeneity is poor, magnetic content unstable, magnetic is more weak, it is desirable to provide the preparation method of a kind of temperature sensitive magnetic high hydroscopic resin overcoming the problems referred to above.Temperature sensitive magnetic water-absorbing resin is utilized to have water imbibition, temperature sensitive and magnetic concurrently, use it for removing fine mineral moisture, after resin and fine mineral mixed dehydration, by magnetic separation method, temperature sensitive magnetic water-absorbing resin is separated from fine mineral, can be recycled after being dehydrated with non-phase transformation by temperature change.The present invention is achieved through the following technical solutions: a kind of fine mineral is dehydrated the preparation method of temperature sensitive magnetic high hydroscopic resin, comprises the steps:
(1) with raw material FeSO4∙7H2O and Fe (NO3)3∙9H2O is respectively configured the solution that concentration is 0.5-1.2mol/L; it is added dropwise in same container with the ammonia spirit that concentration is 1.0-2.5mol/L simultaneously; three's molar ratio is 1:1:1.5-1:3:3, and heating water bath 40-90 DEG C, stirred under nitrogen atmosphere forms colloidal solution in 1-2 hour;
Under nitrogen protection, organic media and water are mixed with volume ratio 10:1-10:6, is subsequently adding above-mentioned colloidal solution and is uniformly mixed, FeSO in mixed solution4∙7H2O and Fe (NO3)3∙9H2The quality sum of O and the mass ratio of organic media are 3:100-7:30, add PAA, acrylic acid, crosslinking agent, initiator stirring the most under agitation, react 0.5-1.0 hour heating water bath 10-90 DEG C;Described PAA is 1:3-1:10 with the mass ratio of organic media;Described PAA and acrylic acid mass ratio are 1:0.1-1:0.5;Crosslinking agent described in this step is 0.01:1-0.03:1 with the mass ratio of PAA;Initiator described in this step is 0.03:1-0.07:1 with the mass ratio of PAA;
(2) forming temperature sensitive monomer solution after temperature sensitive monomer being dissolved, its medium that dissolves used is water, ethanol or water and alcohol mixed solvent, is then added by temperature sensitive monomer solution in the reaction system of step (1);Dissolving medium and use water and during alcohol mixed solvent, wherein volume ratio both water and ethanol is 1:1-1:4;Described temperature sensitive monomer with dissolve mass of medium ratio for 0.1:1-0.5:1;Described temperature sensitive monomer is 0.5:1-1.5:1 with the mass ratio of PAA;
Add crosslinking agent, initiator, stirring, and react 1-6 hour heating water bath 10-50 DEG C;Crosslinking agent described in this step is 0.02:1-0.06:1 with the mass ratio of PAA;Initiator described in this step is 0.06:1-0.15:1 with the mass ratio of PAA;
(3) finally being separated under the suction of magnet by step (2) products obtained therefrom, products therefrom is vacuum dried and i.e. obtains product afterwards.
Further, the raw material FeSO described in step (1)4∙7H2O and Fe (NO3)3∙9H2O gross mass is 0.3:1-0.7:1 with the mass ratio of PAA.
Further, the organic media described in step (1) is any one or the mixture of any two kinds in hexamethylene, normal heptane, ethylbenzene, dimethylbenzene;When using two kinds of organic medias, the volume ratio of the two is 1:1-1:5;This statement refers to, optional two kinds of independent assortments in hexamethylene, normal heptane, ethylbenzene, dimethylbenzene, and all can use this volume ratio.
Further, temperature sensitive monomer described in step (2) is NIPA, methylcellulose, hydroxy propyl cellulose, polyvinyl alcohol, vinyl acetate, N, any one or the mixture of any two kinds of monomers in N-acrylamide, expoxy propane, oxirane, styrene, when using two kinds of materials, the two mass ratio is 3:1-5:1;This statement refers to: when being elected to above-mentioned any two kinds of material independent assortments, all can use this mass ratio.
Further, the crosslinking agent described in step (1) is divinylbenzene, diisocyanate, N, any one in N-methylene-bisacrylamide.
Further, any one during the initiator described in step (1) is azo-bis-iso-dimethyl, azo diisopropyl imidazoline hydrochloric acid potassium, ammonium persulfate, benzoyl peroxide.
Further, the crosslinking agent described in step (2) is any one in hydroxy-ethyl acrylate, hydroxypropyl acrylate, methacrylic acid, hydroxyethyl methacrylate, hydroxy propyl methacrylate, divinylbenzene, N hydroxymethyl acrylamide, DAAM.
Further, any one during the initiator described in step (2) is azo-bis-iso-dimethyl, azo diisopropyl imidazoline hydrochloric acid potassium, ammonium persulfate.
Fine mineral described in step (3) is dehydrated the lowest critical solution temperature of temperature sensitive magnetic high hydroscopic resin and is 30-50 DEG C.
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 add resin monomer, temperature sensitive raw material, crosslinking agent and initiator, magnetic ferroferric oxide is formed the most firm parcel, the problem that magnetic homogeneity is poor, magnetic content is low, magnetic is more weak that existing preparation magnetic water-absorbing resin exists can be overcome;Make resin have high-hydroscopicity, Thermo-sensitive and magnetic simultaneously, utilize its characteristic, both can complete the resin high-efficiency dehydration to fine mineral, the recycling of resin can be realized again with comparalive ease.
Accompanying drawing explanation
Fig. 1 is the Magnetic Test result schematic diagram of specific embodiment of the invention gained sample.
Fig. 2 is the SEM photograph of specific embodiment of the invention gained sample.
Fig. 3 is the Thermo-sensitive measurement result schematic diagram of specific embodiment of the invention gained sample.
Detailed description of the invention
A kind of fine mineral is dehydrated the preparation method of temperature sensitive magnetic high hydroscopic resin, comprises the steps:
(1) with raw material FeSO4∙7H2O and Fe (NO3)3∙9H2It is that 0.5-1.2mol/L(can use 0.5 mol/L that O is respectively configured concentration, 0.7 mol/L, 1.2 mol/L, 1.0 mol/L) solution, it is that 1.0-2.5mol/L(can use 1.0 mol/L with concentration, 1.5 mol/L, 2.0 mol/L, ammonia spirit 2.5mol/L) is added dropwise in same container simultaneously, three's molar ratio is that 1:1:1.5-1:3:3(may select 1:1:1.5, 1:1.5:2.5, 1:3:3), heating water bath 40-90 DEG C (optional 70 DEG C, 40 DEG C, 50 DEG C, 60 DEG C, 80 DEG C, 90 DEG C), stirred under nitrogen atmosphere forms colloidal solution in 1-2 hour;
Under nitrogen protection, organic media and water be may select 10:2,10:1,10:3,10:6,10:5,10:4 with volume ratio 10:1-10:6() mixing, it is subsequently adding above-mentioned colloidal solution and is uniformly mixed, FeSO in mixed solution4∙7H2O and Fe (NO3)3∙9H2The quality sum of O and the mass ratio of organic media are that 3:100-7:30(may select 3:100,5:50,7:30), add PAA, acrylic acid, crosslinking agent, initiator stirring the most under agitation, heating water bath 10-90 DEG C (optional 30 DEG C, 50 DEG C, 90 DEG C, 70 DEG C, 10 DEG C) reaction 0.5-1.0 hour;Described PAA is that 1:3-1:10(may select 1:9,1:10,1:3,1:5,1:7 with the mass ratio of organic media);Described PAA and acrylic acid mass ratio are that 1:0.1-1:0.5(may select 1:0.3,1:0.1,1:0.5);Crosslinking agent described in this step is that 0.01:1-0.03:1(may select 0.01:1,0.02:1,0.03:1 with the mass ratio of PAA);Initiator described in this step is that 0.03:1-0.07:1(may select 0.03:1,0.05:1,0.07:1 with the mass ratio of PAA);
(2) forming temperature sensitive monomer solution after temperature sensitive monomer being dissolved, its medium that dissolves used is water, ethanol or water and alcohol mixed solvent, is then added by temperature sensitive monomer solution in the reaction system of step (1);Dissolving medium and use water and during alcohol mixed solvent, wherein volume ratio both water and ethanol is that 1:1-1:4(may select 1:1,1:3,1:2,1:4);Described temperature sensitive monomer with dissolve mass of medium ratio for 0.1:1-0.5:1(0.1:1,0.5:1,0.4:1,0.3:1,0.2:1);Described temperature sensitive monomer is that 0.5:1-1.5:1(may select 1.5:1,0.5:1,0.7:1,0.9:1,1.1:1,1.3:1 with the mass ratio of PAA);
Add crosslinking agent, initiator, stirring, and in heating water bath 10-50 DEG C (optional 30 DEG C, 20 DEG C, 40 DEG C, 50 DEG C, 10 DEG C) reaction 1-6 hour (optional 2,3,5,4,6 hours);Crosslinking agent described in this step is that 0.02:1-0.06:1(may select 0.03:1,0.06:1,0.04:1,0.05:1,0.02:1 with the mass ratio of PAA);Initiator described in this step is that 0.06:1-0.15:1(may select 0.09:1,0.06:1,0.12:1,0.15:1 with the mass ratio of PAA);
(3) finally being separated under the suction of magnet by step (2) products obtained therefrom, products therefrom is vacuum dried and i.e. obtains product afterwards.
Raw material FeSO described in step (1)4∙7H2O and Fe (NO3)3∙9H2O gross mass is that 0.3:1-0.7:1(may select 0.3:1,0.5:1,0.7:1 with the mass ratio of PAA).
Organic media described in step (1) is any one or the mixture of any two kinds in hexamethylene, normal heptane, ethylbenzene, dimethylbenzene;When using two kinds of organic medias, the volume ratio of the two is that 1:1-1:5(may select 1:1,1:1.2,1:1.5,1:1.3,1:1.4).
Temperature sensitive monomer described in step (2) is NIPA, methylcellulose, hydroxy propyl cellulose, polyvinyl alcohol, vinyl acetate, N, any one or the mixture of any two kinds of monomers in N-acrylamide, expoxy propane, oxirane, styrene, when using two kinds of materials, the two mass ratio is that 3:1-5:1(may select 3:1,4:1,5:1).
Crosslinking agent described in step (1) is any one in divinylbenzene, diisocyanate, N,N methylene bis acrylamide.
Initiator described in step (1) is any one in azo-bis-iso-dimethyl, azo diisopropyl imidazoline hydrochloric acid potassium, ammonium persulfate, benzoyl peroxide.
Crosslinking agent described in step (2) is any one in hydroxy-ethyl acrylate, hydroxypropyl acrylate, methacrylic acid, hydroxyethyl methacrylate, hydroxy propyl methacrylate, divinylbenzene, N hydroxymethyl acrylamide, DAAM.
Initiator described in step (2) is any one in azo-bis-iso-dimethyl, azo diisopropyl imidazoline hydrochloric acid potassium, ammonium persulfate.
Further illustrate the present invention below by embodiment, but be not limited to following example.
Embodiment 1It is respectively configured the FeSO of molar concentration 0.5mol/L and 1.0mol/L4∙7H2O and Fe (NO3)3∙9H2O solution 10ml, is simultaneously added dropwise with 2.0mol/L ammonia spirit 15ml, and heating water bath 60 DEG C, stirred under nitrogen atmosphere forms colloidal solution in 1 hour.
Under nitrogen protection; 50ml hexamethylene, 25ml ethylbenzene and 20ml water are simultaneously introduced above-mentioned sol solution and are uniformly mixed; the most once add 8g PAA, 2g acrylic acid, 0.08g crosslinking agent N; N-methylene-bisacrylamide, 0.24g initiator ammonium persulfate, react 0.5 hour heating water bath 50 DEG C.
4g NIPA is dissolved in 20ml water, is subsequently added into above-mentioned reaction system, be eventually adding 0.2g crosslinking agent hydroxy-ethyl acrylate and 0.5g initiator azo-bis-iso-dimethyl, stirring, then react 2 hours heating water bath 40 DEG C.Products therefrom is vacuum dried, and ferroso-ferric oxide content is 33% after measured, its saturation magnetization 123emu/g(such as Fig. 1 a), under room temperature, water absorption rate (SR) is up to 972g/g, and lowest critical solution temperature (LCST) is 32 DEG C (such as Fig. 3 a).
Embodiment 2It is respectively configured the FeSO of molar concentration 1.0mol/L and 1.0mol/L4∙7H2O and Fe (NO3)3∙9H2O solution 10ml, is simultaneously added dropwise with 2.5mol/L ammonia spirit 20ml, and heating water bath 80 DEG C, stirred under nitrogen atmosphere forms colloidal solution in 2 hours.
Under nitrogen protection; 100ml hexamethylene and 10ml water are simultaneously introduced above-mentioned sol solution and are uniformly mixed; the most once add 20g PAA, 8g acrylic acid, 0.4g crosslinking agent diisocyanate, 0.8g initiator azo diisopropyl imidazoline hydrochloric acid potassium, react 1.0 hours heating water bath 30 DEG C.
14g NIPA and 6g oxirane are dissolved in 180ml water, are subsequently added into above-mentioned reaction system, be eventually adding 1.0g crosslinking agent methacrylic acid and 1.5g initiator ammonium persulfate, stirring, then react 4 hours heating water bath 50 DEG C.Products therefrom is vacuum dried, and ferroso-ferric oxide content is 27% after measured, its saturation magnetization 75emu/g(such as Fig. 1 b), under room temperature, water absorption rate (SR) is up to 650g/g, and lowest critical solution temperature (LCST) is 42 DEG C (such as Fig. 3 b).
Water absorption rate can be at 500-972 g/g, at 70-123 emu/g. SEM photograph, magnetic can show that the magnetic-particle synthesizing temperature sensitive magnetic water-absorbing resin is evenly distributed.Fig. 2 a is the SEM photograph of embodiment 1 products obtained therefrom, and Fig. 2 b is the SEM photograph of embodiment 2 products obtained therefrom.

Claims (10)

1. the preparation method of the fine mineral temperature sensitive magnetic high hydroscopic resin of dehydration, it is characterised in that comprise the steps:
(1) with raw material FeSO4∙7H2O and Fe (NO3)3∙9H2O is respectively configured the solution that concentration is 0.5-1.2mol/L; it is added dropwise in same container with the ammonia spirit that concentration is 1.0-2.5mol/L simultaneously; three's molar ratio is 1:1:1.5-1:3:3, and heating water bath 40-90 DEG C, stirred under nitrogen atmosphere forms colloidal solution in 1-2 hour;
Under nitrogen protection, organic media and water are mixed with volume ratio 10:1-10:6, is subsequently adding above-mentioned colloidal solution and is uniformly mixed, FeSO in mixed solution4∙7H2O and Fe (NO3)3∙9H2The quality sum of O and the mass ratio of organic media are 3:100-7:30, add PAA, acrylic acid, crosslinking agent, initiator stirring the most under agitation, react 0.5-1.0 hour heating water bath 10-90 DEG C;Described PAA is 1:3-1:10 with the mass ratio of organic media;Described PAA and acrylic acid mass ratio are 1:0.1-1:0.5;Crosslinking agent described in this step is 0.01:1-0.03:1 with the mass ratio of PAA;Initiator described in this step is 0.03:1-0.07:1 with the mass ratio of PAA;
(2) forming temperature sensitive monomer solution after temperature sensitive monomer being dissolved, its medium that dissolves used is water, ethanol or water and alcohol mixed solvent, is then added by temperature sensitive monomer solution in the reaction system of step (1);Dissolving medium and use water and during alcohol mixed solvent, wherein volume ratio both water and ethanol is 1:1-1:4;Described temperature sensitive monomer with dissolve mass of medium ratio for 0.1:1-0.5:1;Described temperature sensitive monomer is 0.5:1-1.5:1 with the mass ratio of PAA;
Add crosslinking agent, initiator, stirring, and react 1-6 hour heating water bath 10-50 DEG C;Crosslinking agent described in this step is 0.02:1-0.06:1 with the mass ratio of PAA;Initiator described in this step is 0.06:1-0.15:1 with the mass ratio of PAA;
(3) finally being separated under the suction of magnet by step (2) products obtained therefrom, products therefrom is vacuum dried and i.e. obtains product afterwards.
A kind of fine mineral the most according to claim 1 is dehydrated the preparation method of temperature sensitive magnetic high hydroscopic resin, it is characterised in that: the raw material FeSO described in step (1)4∙7H2O and Fe (NO3)3∙9H2O gross mass is 0.3:1-0.7:1 with the mass ratio of PAA.
A kind of fine mineral the most according to claim 1 and 2 is dehydrated the preparation method of temperature sensitive magnetic high hydroscopic resin, it is characterised in that: the organic media described in step (1) is any one or the mixture of any two kinds in hexamethylene, normal heptane, ethylbenzene, dimethylbenzene;When using two kinds of organic medias, the volume ratio of the two is 1:1-1:5.
A kind of fine mineral the most according to claim 1 and 2 is dehydrated the preparation method of temperature sensitive magnetic high hydroscopic resin, it is characterized in that: the temperature sensitive monomer described in step (2) is NIPA, methylcellulose, hydroxy propyl cellulose, polyvinyl alcohol, vinyl acetate, N, any one or the mixture of any two kinds in N-acrylamide, expoxy propane, oxirane, styrene;When using two kinds of materials, the two mass ratio is 3:1-5:1.
A kind of fine mineral the most according to claim 1 and 2 is dehydrated the preparation method of temperature sensitive magnetic high hydroscopic resin, it is characterized in that: the crosslinking agent described in step (1) is divinylbenzene, diisocyanate, N, any one in N-methylene-bisacrylamide.
A kind of fine mineral the most according to claim 1 and 2 is dehydrated the preparation method of temperature sensitive magnetic high hydroscopic resin, it is characterised in that: the initiator described in step (1) is any one in azo-bis-iso-dimethyl, azo diisopropyl imidazoline hydrochloric acid potassium, ammonium persulfate, benzoyl peroxide.
A kind of fine mineral the most according to claim 1 and 2 is dehydrated the preparation method of temperature sensitive magnetic high hydroscopic resin, it is characterised in that: the crosslinking agent described in step (2) is any one in hydroxy-ethyl acrylate, hydroxypropyl acrylate, methacrylic acid, hydroxyethyl methacrylate, hydroxy propyl methacrylate, divinylbenzene, N hydroxymethyl acrylamide, DAAM.
A kind of fine mineral the most according to claim 3 is dehydrated the preparation method of temperature sensitive magnetic high hydroscopic resin, it is characterised in that: the crosslinking agent described in step (2) is any one in hydroxy-ethyl acrylate, hydroxypropyl acrylate, methacrylic acid, hydroxyethyl methacrylate, hydroxy propyl methacrylate, divinylbenzene, N hydroxymethyl acrylamide, DAAM.
A kind of fine mineral the most according to claim 1 and 2 is dehydrated the preparation method of temperature sensitive magnetic high hydroscopic resin, it is characterised in that: the initiator described in step (2) is any one in azo-bis-iso-dimethyl, azo diisopropyl imidazoline hydrochloric acid potassium, ammonium persulfate.
A kind of fine mineral the most according to claim 3 is dehydrated the preparation method of temperature sensitive magnetic high hydroscopic resin, it is characterised in that: the initiator described in step (2) is any one in azo-bis-iso-dimethyl, azo diisopropyl imidazoline hydrochloric acid potassium, ammonium persulfate.
CN201610163954.3A 2016-03-22 2016-03-22 A kind of fine mineral is dehydrated the preparation method of temperature sensitive magnetic high hydroscopic resin Expired - Fee Related CN105777974B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610163954.3A CN105777974B (en) 2016-03-22 2016-03-22 A kind of fine mineral is dehydrated the preparation method of temperature sensitive magnetic high hydroscopic resin

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610163954.3A CN105777974B (en) 2016-03-22 2016-03-22 A kind of fine mineral is dehydrated the preparation method of temperature sensitive magnetic high hydroscopic resin

Publications (2)

Publication Number Publication Date
CN105777974A true CN105777974A (en) 2016-07-20
CN105777974B CN105777974B (en) 2017-08-25

Family

ID=56390435

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610163954.3A Expired - Fee Related CN105777974B (en) 2016-03-22 2016-03-22 A kind of fine mineral is dehydrated the preparation method of temperature sensitive magnetic high hydroscopic resin

Country Status (1)

Country Link
CN (1) CN105777974B (en)

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
宫艺等: "聚( N-异丙基丙烯酰胺-co-丙烯酸) / Fe3O4复合微球的制备及表征", 《高分子材料科学与工程》 *

Also Published As

Publication number Publication date
CN105777974B (en) 2017-08-25

Similar Documents

Publication Publication Date Title
Ma et al. Synthesis and characterization of micron‐sized monodisperse superparamagnetic polymer particles with amino groups
Jiang et al. Magnetic ATP/FA/Poly (AA-co-AM) ternary nanocomposite microgel as selective adsorbent for removal of heavy metals from wastewater
CN102641753B (en) Method for preparing magnetic strong-basicity ion exchange resin for removing organic matters in water
CN105107482A (en) Preparation method for molecular imprinting material and molecular imprinting material prepared through preparation method
EP2424901A1 (en) Monodisperse submicron polymer particles
RU98103394A (en) MAGNETIC POLYMER PARTICLES BASED ON POLYVINYL ALCOHOL, METHODS FOR PRODUCING AND APPLICATION
CN104353435B (en) Nitrogen heterocyclic ring compound modified magnetic polystyrene microsphere, preparation method and application thereof
CA2679542A1 (en) Imprinted polymers
Mao et al. Well-defined sulfamethazine-imprinted magnetic nanoparticles via surface-initiated atom transfer radical polymerization for highly selective enrichment of sulfonamides in food samples
Qin et al. Rapid and selective extraction of multiple sulfonamides from aqueous samples based on Fe 3 O 4–chitosan molecularly imprinted polymers
CN102489273B (en) Preparation method of magnetic beads of dendritic molecular imprinting polymer on surface of estrogenic nano silica gel
Chen et al. Magnetic molecularly imprinted polymers synthesized by surface‐initiated reversible addition‐fragmentation chain transfer polymerization for the enrichment and determination of synthetic estrogens in aqueous solution
CN104387712A (en) Nano composite carrier with superparamagnetism and preparation method thereof
Phutthawong et al. Facile synthesis of magnetic molecularly imprinted polymers for caffeine via ultrasound-assisted precipitation polymerization
CN104130441B (en) Magnetic field-induced preparation method of molecularly-imprinted magnetic enrichment material of trace quantity of chlorophenol pollutant molecules in seawater
CN106753079A (en) The preparation method of nanometer ferroferric oxide modification water-and acrylate magnetic pressure sensitive adhesive
CN105777974A (en) Preparation method of temperature-sensitive magnetic high-hygroscopicity resin for fine mineral dewatering
CN102746440B (en) Preparation technology of polystyrene microsphere for reinforcing turbidimetric reagent
CN104087286A (en) Polymer pH fluorescent probe PRBH, and preparation method and application thereof
Zou et al. Magnetic and hydrophilic imprinted particles via ATRP at room temperature for selective separation of sulfamethazine
CN103804699A (en) Cassava starch magnetic microsphere and preparation method thereof
CN105693918B (en) A kind of preparation method of magnetic hollow structural molecule imprinted polymer
CN103012815A (en) Method for preparing narrow-dispersion high-magnetic chitosan sub-micron particles
CN105597657A (en) Functional composite metal oxide material, preparation method and application thereof
CN111116851A (en) Preparation method of polyquaternium magnetic microsphere with core-shell structure

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20170825

Termination date: 20200322