CN103819856A - Sodium polyacrylate in-situ growing prussian blue nanocrystalline composite, and preparation method and application thereof - Google Patents
Sodium polyacrylate in-situ growing prussian blue nanocrystalline composite, and preparation method and application thereof Download PDFInfo
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- CN103819856A CN103819856A CN201410057889.7A CN201410057889A CN103819856A CN 103819856 A CN103819856 A CN 103819856A CN 201410057889 A CN201410057889 A CN 201410057889A CN 103819856 A CN103819856 A CN 103819856A
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Abstract
The invention relates to a sodium polyacrylate in-situ growing prussian blue nanocrystalline composite, and a preparation method and an application thereof. The invention relates to a nanocomposite, and a preparation method and an application thereof. The invention aims to solve the problems that a conventional composite preparation process is complex; nanoparticles are easy to agglomerate; and plussian blue content is low and the composite is easy to fall off. The composite provided by the invention is prepared from 40%-90% of iron polyacrylate and 10%-60% of prussian blue. A method comprises the steps of 1. dissolving a trivalent iron salt in a mixed solution of deionized water and glacial acetic acid; 2. adding sodium polyacrylate; and 3. adding K4[Fe(CN)6] or Na4[Fe(CN)6]. The composite provided by the invention is used for preparing sodium polyacrylate in-situ growing prussian blue nanocrystalline composite foam polyurethane sponge.
Description
Technical field
The present invention relates to nano composite material and its preparation method and application, belong to advanced nano composite material and environment remediation technical field.
Background technology
The stable development of Nuclear Power Industry provides effective way for solving world energy sources crisis, but also brings potential nuclear radiation to pollute secret worry.It is maximum safety and environmental protection hidden danger in current known nuclear energy application that the nuclear radiation that nuclear leakage causes is polluted.Research shows, nuclear pollution composition comprises the multiple radioelement such as caesium (Cs-131,133,137), strontium (Sr90) and iodine (I-131,135), wherein radiocesium (12.8%, the transformation period is about 30 years) is one of for main component.Also adopting the general treatment process of polluting and administer for nuclear pollution, such as: 1, soil moved in to improve the original method, replace by heavily contaminated; 2, electrochemical rehabilitation; 3, ion-exchange, flocculation sediment; 4, phytoremediation; 5, the method such as restoration of the ecosystem.These methods exist periodically long, and eurytropy is poor, and high cost is repaired the shortcomings such as not thorough and inefficiency.For problems and the shortcoming of existing nuclear radiation pollution treatment method, find a kind of simple, safe method extremely urgent with the research of the radioactive substance in purifying waste water or in soil.Nano material, compared with traditional material, has brand-new good physical/chemical properties, and studied person's extensive concern and expectation.
As everyone knows, Prussian blue (Prussian blue, PB) be a kind of cheapness, high stability, caesium is had to highly selective adsorptive power, the complicated coordination compound of the blueness of synthetic is used to the sorbent material of the radiocesium of removing human or animal's picked-up all the time.But, PB crystal very little (the PB monocrystalline length of side is only 1.02nm in theory), such minicrystal for absorption after, filter or the method such as centrifugal to do recycling be very difficult.In recent years, composite organic-inorganic material Yin Qiyi reclaims, and can solve the shortcoming that nano material is easily assembled, and gives full play to the excellent properties of nano material and becomes a kind of advanced composite material with wide application prospect.But up to the present, the synthetic and application of sodium polyacrylate growth in situ prussian blue nano crystal composite material have not been reported.
In existing report, the matrix material of synthesized has complicated process of preparation, and nanoparticle is easily reunited, and Prussian blue content is low, is easy to come off etc. not enough.
Summary of the invention
The object of the invention is in order to solve existing composite material preparation process complexity, nanoparticle is easily reunited, and Prussian blue content is low, and the problem that is easy to come off provides sodium polyacrylate growth in situ prussian blue nano crystal composite material and its preparation method and application.
Sodium polyacrylate growth in situ prussian blue nano crystal composite material of the present invention is by polyacrylic acid iron and Prussian blue making, and wherein, the quality percentage composition of polyacrylic acid iron is 40%～90%, and Prussian blue quality percentage composition is 10%～60%.
The preparation method of sodium polyacrylate growth in situ prussian blue nano crystal composite material of the present invention, realizes by following steps:
One, according to mole with volume ratio 1mmol:(15mL～35mL) ratio trivalent iron salt is dissolved under agitation condition in the mixing solutions of deionized water and Glacial acetic acid, stir 0.5h～2h, obtain solution; Wherein the volume ratio of deionized water and Glacial acetic acid is 1mL:(0.5mL～1mL);
Two, in the solution obtaining to step 1, add sodium polyacrylate, make Fe
3+with Na
+mol ratio be 1:(2～3), continue to stir standing separation after 48h～96h, collect pressed powder, then use deionized water wash pressed powder 3～6 times, after filtration, regather pressed powder;
Three, in the pressed powder obtaining to step 2, add with step 1 in deionized water and the isopyknic deionized water of mixing solutions of Glacial acetic acid, then under agitation condition, add K
4[Fe (CN)
6] or Na
4[Fe (CN)
6], make Fe
3+with [Fe (CN)
6]
4-mol ratio be 1:(0.5～0.75), standing separation after stirring 20min～60min, the pressed powder obtaining with deionized water wash separation 3～6 times is then dried pressed powder at 30 ℃～80 ℃, completes the preparation of sodium polyacrylate growth in situ prussian blue nano crystal composite material.
Wherein, above-mentioned sodium polyacrylate used is the commercially available particulate of molecular weight more than 3000, obtains by purchase.
Sodium polyacrylate growth in situ prussian blue nano crystal composite material of the present invention is for the preparation of sodium polyacrylate growth in situ prussian blue nano crystal composite material polyurathamc sponge.
Beneficial effect of the present invention:
1, the invention provides the preparation method of a kind of netted sodium polyacrylate growth in situ prussian blue nano crystal composite material (SP/PB) and polyurathamc sponge (SP/PB-PUF) thereof, synthesize prussian blue nano crystal multilevel hierarchy matrix material by competitive coordination reaction at polymkeric substance internal in-situ, again by compound to matrix material and polyurathamc, prepare the efficient of selective adsorption caesium, simple to operate, eurytopic three-dimensional novel practical portable type nuclear pollution scavenging material-polyurathamc sponge, combine highly selective and the polymkeric substance high molecular easy recyclability of prussian blue nano crystal to cesium ion, have wide practical use in environmental pollution reparation field,
2, the sodium polyacrylate growth in situ prussian blue nano crystal composite material that prepared by the present invention, is take the three-dimensional netted polymkeric substance of sodium polyacrylate as parent, utilizes the abundant oxy radical of sodium polyacrylate, by Fe
3+catch in polymer network structure, synthesize prussian blue nano crystal multilevel hierarchy matrix material by growth in situ self-assembling technique at polymkeric substance internal in-situ, synthetic sodium polyacrylate/Prussian blue matrix material size is between 1～10 μ m, prussian blue nano crystalline substance is between 10～200nm, nanoparticle is uniformly dispersed, Prussian blue content high (being about 10%～60%), difficult drop-off;
3, sodium polyacrylate/Prussian blue polyurathamc sponge matrix material that prepared by the present invention, with sodium polyacrylate/Prussian blue matrix material, to be furnished with micro-surfactant, the SP/PB aqueous solution and polyurathamc (as NB-9000B) under high-speed stirring, (be greater than 2000rpm/min) foaming polymerization, SP/PB is fixed on the cell wall (Cell wall) of polyurethane foam the most at last, obtains spongy SP/PB-PUF sorbing material;
4, the material of reporting before sodium polyacrylate growth in situ prussian blue nano crystal composite material prepared by the present invention and polyurathamc sponge thereof are different from, polymkeric substance polymer material molding is good, growth in situ has given Prussian blue good dispersiveness, polyurathamc sponge has good permeability, the inventive method takes full advantage of the macroscopic property of forming polymer, having raw material is easy to get, synthetic method is simply rapid, separate easy, be suitable for scale operation and engineering application, due to its easy separation and high caesium selectivity, there is important application prospect in fields such as nuclear pollution processing,
5, sodium polyacrylate growth in situ prussian blue nano crystal composite material and the polyurathamc sponge thereof that prepared by the present invention, in polyurathamc sponge, the content of SP/PB can be controlled between 0～25%, for the reparation of the cesium ion contaminate environment such as water body, soil, atmosphere, in middle low contaminate environment, the clearance of caesium can reach more than 90%.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of 10000 times of the sodium polyacrylate growth in situ prussian blue nano crystal composite materials prepared of embodiment mono-;
Fig. 2 is the scanning electron microscope (SEM) photograph of 500 times of the sodium polyacrylate growth in situ prussian blue nano crystal composite materials prepared of embodiment mono-;
Fig. 3 is the projection Electronic Speculum figure of 71000 times of the sodium polyacrylate growth in situ prussian blue nano crystal composite materials prepared of embodiment mono-.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: present embodiment sodium polyacrylate growth in situ prussian blue nano crystal composite material is by polyacrylic acid iron and Prussian blue making, wherein, the quality percentage composition of polyacrylic acid iron is 40%～90%, and Prussian blue quality percentage composition is 10%～60%.
The beneficial effect of present embodiment:
Sodium polyacrylate growth in situ prussian blue nano crystal composite material prepared by present embodiment, is take the three-dimensional netted polymkeric substance of sodium polyacrylate as parent, utilizes the abundant oxy radical of sodium polyacrylate, by Fe
3+catch in polymer network structure, synthesize prussian blue nano crystal multilevel hierarchy matrix material by growth in situ self-assembling technique at polymkeric substance internal in-situ, synthetic sodium polyacrylate/Prussian blue matrix material size is between 1～10 μ m, prussian blue nano crystalline substance is between 10～200nm, nanoparticle is uniformly dispersed, Prussian blue content high (being about 10%～60%), difficult drop-off.
Embodiment two: the preparation method of present embodiment sodium polyacrylate growth in situ prussian blue nano crystal composite material, carries out according to the following steps:
One, according to mole with volume ratio 1mmol:(15mL～35mL) ratio trivalent iron salt is dissolved under agitation condition in the mixing solutions of deionized water and Glacial acetic acid, stir 0.5h～2h, obtain solution; Wherein the volume ratio of deionized water and Glacial acetic acid is 1mL:(0.5mL～1mL);
Two, in the solution obtaining to step 1, add sodium polyacrylate, make Fe
3+with Na
+mol ratio be 1:(2～3), continue to stir standing separation after 48h～96h, collect pressed powder, then use deionized water wash pressed powder 3～6 times, after filtration, regather pressed powder;
Three, in the pressed powder obtaining to step 2, add with step 1 in deionized water and the isopyknic deionized water of mixing solutions of Glacial acetic acid, then under agitation condition, add K
4[Fe (CN)
6] or Na
4[Fe (CN)
6], make Fe
3+with [Fe (CN)
6]
4-mol ratio be 1:(0.5～0.75), standing separation after stirring 20min～60min, the pressed powder obtaining with deionized water wash separation 3～6 times is then dried pressed powder at 30 ℃～80 ℃, completes the preparation of sodium polyacrylate growth in situ prussian blue nano crystal composite material.
The beneficial effect of present embodiment:
Sodium polyacrylate growth in situ prussian blue nano crystal composite material polymkeric substance polymer material molding prepared by present embodiment is good, growth in situ has given Prussian blue good dispersiveness, present embodiment method takes full advantage of the macroscopic property of forming polymer, have that raw material is easy to get, synthetic method is simple rapidly, it is easy to separate, and is suitable for scale operation and engineering application.
Embodiment three: present embodiment is different from embodiment two: described in step 1 according to mole with volume ratio 1mmol:(20mL～30mL) ratio trivalent iron salt is dissolved in the mixing solutions of deionized water and Glacial acetic acid under agitation condition.Other is identical with embodiment two.
Embodiment four: present embodiment is different from embodiment two or three: add sodium polyacrylate in the solution obtaining to step 1 described in step 2, make Fe
3+with Na
+mol ratio be 1:(2.2～2.8).Other is identical with embodiment two or three.
Embodiment five: present embodiment is different from one of embodiment two to four: add again K under the agitation condition described in step 3
4[Fe (CN)
6] or Na
4[Fe (CN)
6], make Fe
3+with [Fe (CN)
6]
4-mol ratio be 1:(0.55～0.7).Other is identical with one of embodiment two to four.
Embodiment six: present embodiment is different from one of embodiment two to five: standing separation after the stirring 20min described in step 3.Other is identical with one of embodiment two to five.
Embodiment seven: present embodiment is different from one of embodiment two to six: pressed powder is dried at 40 ℃ described in step 3.Other is identical with one of embodiment two to six.
Embodiment eight: the application of present embodiment sodium polyacrylate growth in situ prussian blue nano crystal composite material, is characterized in that sodium polyacrylate growth in situ prussian blue nano crystal composite material is for the preparation of sodium polyacrylate growth in situ prussian blue nano crystal composite material polyurathamc sponge.
The beneficial effect of present embodiment:
Sodium polyacrylate/Prussian blue polyurathamc sponge matrix material prepared by present embodiment is with sodium polyacrylate/Prussian blue matrix material, to be furnished with micro-surfactant, the SP/PB aqueous solution and polyurathamc (as NB-9000B) under high-speed stirring, (be greater than 2000rpm/min) foaming polymerization, SP/PB is fixed on the cell wall (Cell wall) of polyurethane foam the most at last, obtains spongy SP/PB-PUF sorbing material.
Sodium polyacrylate growth in situ prussian blue nano crystal composite material polyurathamc sponge prepared by present embodiment, for the reparation of the cesium ion contaminate environment such as water body, soil, atmosphere, in middle low contaminate environment, the clearance of caesium can reach more than 90%.
Embodiment nine: present embodiment is different from embodiment eight: described sodium polyacrylate growth in situ prussian blue nano crystal composite material, for the preparation of sodium polyacrylate growth in situ prussian blue nano crystal composite material polyurathamc sponge, carries out according to following steps:
Sodium polyacrylate growth in situ prussian blue nano crystal composite material is scattered in the aqueous solution that contains surfactant under stirring ultrasound condition, wherein the mass volume ratio of matrix material and surfactant, water is 1g:(0.1mL～0.2mL): (20mL～50mL), then the mixture obtaining and isopyknic NB-9000B are greater than to the polymerization of foaming under the agitation condition of 2000rpm/min at rotating speed, dry at 30 ℃～80 ℃ again, complete the preparation of sodium polyacrylate growth in situ prussian blue nano crystal composite material polyurathamc sponge.Other is identical with embodiment eight.
Embodiment ten: present embodiment is different from embodiment eight or nine: the polymerization of foaming under the described agitation condition that is 2000rpm/min at rotating speed by the mixture obtaining and isopyknic NB-9000B, drier at 40 ℃.Other is identical with embodiment eight or nine.
Embodiment 11: present embodiment is different from one of embodiment eight to ten: described surfactant is commercially available surfactant, obtains by purchase.Other is identical with one of embodiment eight to ten.
Verify beneficial effect of the present invention by following examples:
Embodiment mono-:
The preparation method of the present embodiment sodium polyacrylate growth in situ prussian blue nano crystal composite material, carries out according to the following steps:
One, 1.71g iron(ic) chloride is dissolved under agitation condition in the mixing solutions of 150mL deionized water and 100mL Glacial acetic acid, stirs 0.5h;
Two, in the solution obtaining to step 1, add sodium polyacrylate 1g, standing separation after continuation stirring 48h, collects pressed powder, then separates with deionized water wash the pressed powder 3 times (until solution is colourless) obtaining, and regathers pressed powder;
Three, in the pressed powder obtaining to step 2, add the deionized water of 250mL, under agitation condition, add again 2.6g K
4[Fe (CN)
6], standing separation after stirring 20min, separates the pressed powder 3 times (until solution is colourless) obtaining with deionized water wash, then pressed powder is dried at 40 ℃, completes the preparation of sodium polyacrylate growth in situ prussian blue nano crystal composite material.
Wherein, above-mentioned sodium polyacrylate used is the commercially available particulate of molecular weight more than 3000, obtains by purchase.
The scanning electron microscope (SEM) photograph that sodium polyacrylate growth in situ prussian blue nano crystal composite material prepared by the present embodiment is 10000 times as shown in Figure 1, the scanning electron microscope (SEM) photograph of 500 times as shown in Figure 2, the projection Electronic Speculum figure of 71000 times as shown in Figure 3, result shows that the sodium polyacrylate growth in situ prussian blue nano crystal composite material nanoparticle of preparation is uniformly dispersed, Prussian blue content is high, difficult drop-off.
Embodiment bis-:
The preparation method of the present embodiment sodium polyacrylate growth in situ prussian blue nano crystal composite material, carries out according to the following steps:
One, 1.71g iron(ic) chloride is dissolved under agitation condition in the mixing solutions of 150mL deionized water and 100mL Glacial acetic acid, stirs 0.5h;
Two, in the solution obtaining to step 1, add sodium polyacrylate 3g, standing separation after continuation stirring 48h, collects pressed powder, then separates with deionized water wash the pressed powder 3 times (until solution is colourless) obtaining, and regathers pressed powder;
Three, in the pressed powder obtaining to step 2, add the deionized water of 250mL, under agitation condition, add again 2.6g K
4[Fe (CN)
6], standing separation after stirring 20min, separates the pressed powder 3 times (until solution is colourless) obtaining with deionized water wash, then pressed powder is dried at 40 ℃, completes the preparation of sodium polyacrylate growth in situ prussian blue nano crystal composite material.
Wherein, above-mentioned sodium polyacrylate used is the commercially available particulate of molecular weight more than 3000, obtains by purchase.
Embodiment tri-:
The present embodiment sodium polyacrylate growth in situ prussian blue nano crystal composite material, for the preparation of sodium polyacrylate growth in situ prussian blue nano crystal composite material polyurathamc sponge, carries out according to the following steps:
Sodium polyacrylate growth in situ prussian blue nano crystal composite material 6.5g is scattered in the 60mL aqueous solution under stirring ultrasound condition, take again polyurethane prepolymer NB-9000B120g, add Pluronic L-62(surfactant) 500 μ L, then the polymerization of the matrix material aqueous solution obtaining and polyurethane prepolymer NB-9000B solution being foamed under the agitation condition of 2000rpm/min, dry at 40 ℃ again, complete the preparation of sodium polyacrylate growth in situ prussian blue nano crystal composite material polyurathamc sponge.
Described surfactant is commercially available surfactant Pluronic L-62, obtains by purchase.
Polyacrylic acid iron in polyurathamc sponge prepared by the present embodiment/Prussian blue content is 5%.
The prepared matrix material of above-described embodiment, for the reparation of the cesium ion contaminate environment such as water body, soil, atmosphere, have broad application prospects, and preparation method is simple in nuclear pollution environment remediation field, and raw material is easy to get, and is suitable for amplifying producing.
Claims (10)
1. sodium polyacrylate growth in situ prussian blue nano crystal composite material, it is characterized in that it is by polyacrylic acid iron and Prussian blue making, wherein, the quality percentage composition of polyacrylic acid iron is 40%～90%, and Prussian blue quality percentage composition is 10%～60%.
2. prepare a method for sodium polyacrylate growth in situ prussian blue nano crystal composite material claimed in claim 1, it is characterized in that it carries out according to following steps:
One, according to mole with volume ratio 1mmol:(15mL～35mL) ratio trivalent iron salt is dissolved under agitation condition in the mixing solutions of deionized water and Glacial acetic acid, stir 0.5h～2h, obtain solution; Wherein the volume ratio of deionized water and Glacial acetic acid is 1mL:(0.5mL～1mL);
Two, in the solution obtaining to step 1, add sodium polyacrylate, make Fe
3+with Na
+mol ratio be 1:(2～3), continue to stir standing separation after 48h～96h, collect pressed powder, then use deionized water wash pressed powder 3～6 times, after filtration, regather pressed powder;
Three, in the pressed powder obtaining to step 2, add with step 1 in deionized water and the isopyknic deionized water of mixing solutions of Glacial acetic acid, then under agitation condition, add K
4[Fe (CN)
6] or Na
4[Fe (CN)
6], make Fe
3+with [Fe (CN)
6]
4-mol ratio be 1:(0.5～0.75), standing separation after stirring 20min～60min, the pressed powder obtaining with deionized water wash separation 3～6 times is then dried pressed powder at 30 ℃～80 ℃, completes the preparation of sodium polyacrylate growth in situ prussian blue nano crystal composite material.
3. the preparation method of sodium polyacrylate growth in situ prussian blue nano crystal composite material according to claim 2, it is characterized in that described in step 1 according to mole with volume ratio 1mmol:(20mL～30mL) ratio trivalent iron salt is dissolved in the mixing solutions of deionized water and Glacial acetic acid under agitation condition.
4. the preparation method of sodium polyacrylate growth in situ prussian blue nano crystal composite material according to claim 2, is characterized in that adding sodium polyacrylate in the solution obtaining to step 1 described in step 2, makes Fe
3+with Na
+mol ratio be 1:(2.2～2.8).
5. the preparation method of sodium polyacrylate growth in situ prussian blue nano crystal composite material according to claim 2, is characterized in that adding under the agitation condition described in step 3 K again
4[Fe (CN)
6] or Na
4[Fe (CN)
6], make Fe
3+with [Fe (CN)
6]
4-mol ratio be 1:(0.55～0.7).
6. the preparation method of sodium polyacrylate growth in situ prussian blue nano crystal composite material according to claim 2, is characterized in that standing separation after the stirring 20min described in step 3.
7. the preparation method of sodium polyacrylate growth in situ prussian blue nano crystal composite material according to claim 2, is characterized in that pressed powder is dried at 40 ℃ described in step 3.
8. the application of sodium polyacrylate growth in situ prussian blue nano crystal composite material, is characterized in that sodium polyacrylate growth in situ prussian blue nano crystal composite material is for the preparation of sodium polyacrylate growth in situ prussian blue nano crystal composite material polyurathamc sponge.
9. the application of sodium polyacrylate growth in situ prussian blue nano crystal composite material according to claim 8, it is characterized in that sodium polyacrylate growth in situ prussian blue nano crystal composite material, for the preparation of sodium polyacrylate growth in situ prussian blue nano crystal composite material polyurathamc sponge, carries out according to following steps:
Sodium polyacrylate growth in situ prussian blue nano crystal composite material is scattered in the aqueous solution that contains surfactant under stirring ultrasound condition, wherein the mass volume ratio of matrix material and surfactant, water is 1g:(0.1mL～0.2mL): (20mL～50mL), then the mixture obtaining and isopyknic NB-9000B are greater than to the polymerization of foaming under the agitation condition of 2000rpm/min at rotating speed, dry at 30 ℃～80 ℃ again, complete the preparation of sodium polyacrylate growth in situ prussian blue nano crystal composite material polyurathamc sponge.
10. the application of sodium polyacrylate growth in situ prussian blue nano crystal composite material according to claim 9, the polymerization that it is characterized in that foaming under the described agitation condition that is 2000rpm/min at rotating speed by the mixture obtaining and isopyknic NB-9000B, then be dried at 40 ℃.
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| CN107082438A (en) * | 2017-04-28 | 2017-08-22 | 武汉理工大学 | Prussian blue nano floral structure material and its preparation and application |
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| CN116272900A (en) * | 2023-03-06 | 2023-06-23 | 南开大学 | Prussian blue/polyacrylonitrile composite aerogel material, and preparation method and application thereof |
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