CN100411984C - Method for preparing magnetic granule-attapulgite nano composite material - Google Patents
Method for preparing magnetic granule-attapulgite nano composite material Download PDFInfo
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- CN100411984C CN100411984C CNB2006100401619A CN200610040161A CN100411984C CN 100411984 C CN100411984 C CN 100411984C CN B2006100401619 A CNB2006100401619 A CN B2006100401619A CN 200610040161 A CN200610040161 A CN 200610040161A CN 100411984 C CN100411984 C CN 100411984C
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Abstract
The present invention relates to a preparation method for magnetic particle and attapulgite nanophase composite materials, which is characterized in that attapulgite clay and molysite are used as raw materials; through the nucleus formation on the surface of attapulgite and the stabilization on crystal nucleus of diatomic iron ions or diatomic and teracidic iron ions induced by attapulgite clay, nanometer magnetic particles are directly crystallized from solution and are loaded on the surface of attapulgite crystal to form super paramagnetism particle and attapulgite composite materials. The functional materials with the super paramagnetism characteristic and the strong absorption characteristic can be operated under the action of a magnetic field to realize the magnetic flocculation, the magnetic reclamation, the magnetic filtration and the target control of adsorbing agent. The materials can be widely applied to the purification of industrial raw materials, air purification, depth-type filtration, the feedwater treatment and the advanced treatment of membrane materials, waste water treatment, targeted drug control release, etc.
Description
Technical field:
The present invention relates to a kind of magnetic granule-attapulgite clay composite material preparation method who gives the good magnetic performance of attapulgite clay.
Background technology:
Attapulgite is a kind of moisture zeopan mineral of chain laminate structure, has the rhabdolith form of the about 30nm～40nm of diameter, is a kind of important natural nano-mineral material.Because the attapulgite crystal belongs to the nanoscale characteristic, thereby attapulgite has huge surface-area and adsorption activity, has important potential using value as sorbent material.
Yet, in its application as sorbent material, because attapulgite clay has good colloid property, attapulgite clay has very high colloid-stabilised performance in aqeous suspension, cause solid-liquid separation difficulty in liquid-phase system, this is the difficult problem of restriction attapulgite clay sorbent material industrial applications all the time.Traditional solution route has two kinds, one, the attapulgite clay sorbent material uses with powder type, in order to realize solid-liquid separation, by adding flocculation agent, make the attapulgite clay flocculation sediment. operation by this way, adding flocculation agent increases cost, and the difficulty that sludge quantity is increased considerably with sludge treatment strengthens; Its two, settling mode is to carry out the attapulgite clay granulation, need to add binding agent or pyroprocessing, particle diameter increases, resistance to mass transfer increases, and has reduced the attapulgite clay adsorption effect again, cost is higher simultaneously, the application in some fields is very limited.
Summary of the invention:
The present invention is for avoiding above-mentioned existing in prior technology weak point, the magnetic granule-attapulgite nano composite material that a kind of raw materials consumption is few, technology is simple, production cost is low preparation method is provided, give attapulgite clay good magnetic performance, realize the control of attapulgite sorbent material by electromagnetic field.
The technical scheme that technical solution problem of the present invention is adopted is:
The characteristics of the inventive method are to be raw material with attapulgite clay and molysite, by attapulgite clay inductive divalence or divalence and ferric ion at the attapulgite surface nucleation with to the stabilization of nucleus, make directly crystallization from solution of nano magnetic particle, and load on the attapulgite plane of crystal, constitute supperparamagnetic particles-attapulgite matrix material.
The present invention can also diminish the magnetite crystal particle diameter that direct crystallization forms from solution by adding magnetite crystal growth control agent.
The operation steps of the inventive method is:
A, attapulgite clay impel the brilliant Shu Xieju of attapulgite through the extruding pugging, being made into mass volume ratio with water is 0.1: 100～20: 100 attapulgite clay suspension, preferred solid-to-liquid ratio is 1: 100～5: 100, stirring impels the brilliant bundle of attapulgite to disperse, and forms stable attapulgite clay suspension;
B, operate by one of following dual mode:
Mode one: under agitation condition, add divalent iron salt solution in the attapulgite clay suspension after dispersion treatment, the concentration of iron salt solutions is 1%～50%, preferred concentration is 5%～10%, the mass ratio of iron and attapulgite clay is 100: 0.5～100: 30 in attapulgite clay and the molysite mixed solution, and preferred ratio is 100: 1～100: 5; Attapulgite-molysite mixed solution is heated to 50 ℃～100 ℃, and preferred value is 60 ℃～80 ℃; Be 1%-20% with concentration, preferred concentration is that nitrate and the alkali lye of 5%-10% mixes, and the preparation mixed solution is heated to 50～100 ℃ with the mixed solution of described nitrate and alkali lye, and preferred value is 60 ℃～80 ℃; Described attapulgite-molysite mixed solution is mixed with nitrate-alkali lye mixed solution, and reheat to 50 ℃～100 ℃ stirs aging crystallization 0.5～5 hour; The mol ratio that the nitrate that is added and the amount of alkali lye are controlled at nitrate and molysite is 2: 1～1: 2, and optimum ratio is 1: 1, and the mol ratio of alkali lye and molysite is 2: 1～4: 1, and optimum ratio is 3: 1;
Mode two: under agitation condition, add the mixing solutions of divalent iron salt and trivalent iron salt in the attapulgite clay suspension after dispersion treatment, the concentration of iron salt solutions is 1%～50%, and preferred concentration is 5%～10%; The mol ratio of divalent iron salt and trivalent iron salt is 3: 1～1: 1, and preferred value is 1: 1; It is 0.001-0.1 that control molysite add-on makes iron in the suspension/attapulgite ratio; Under agitation condition, in attapulgite-molysite mixed solution, add alkali lye, the mol ratio of alkali lye and molysite is 4: 1-2: 1; Stir aging crystallization 0.5～5 hour;
C, with suspension dehydration, washing, drying after the aging crystallization of step b, obtain magnetite-attapulgite clay matrix material.Compared with the prior art, beneficial effect of the present invention is embodied in:
That passes through nanoscale discovers that the attapulgite surface can be used as crystallization nucleation center and stable nanoparticles.Thereby, can utilize attapulgite crystal inductive nucleation and nanocrystal stabilizing effect, at the tiny functional particulate of attapulgite area load. form well-proportioned metallic compound-attapulgite clay matrix material, this metallic compound-attapulgite clay nano composite material can be given the various catalytic activitys of attapulgite clay (reactive metals that load is different), conductive characteristic, the strong magnetic properties of super paramagnetic, microwave absorbing property, heat generation characteristic, make the attapulgite clay deep processed product move towards retrofit, deep processing, functionalization, create high added value.
Magnetic granule-attapulgite matrix material with the inventive method preparation, under the prerequisite that keeps attapulgite form, structure, physical and chemical performance, make the attapulgite clay superparamagnetism matrix material of preparation have good absorption property, super paramagnetic characteristic simultaneously.When externally-applied magnetic field, this attapulgite clay superparamagnetism matrix material can be by poles attract; When foreign field was cancelled, because super paramagnetic characteristic, the residual magnetization rate of attapulgite clay superparamagnetism matrix material was zero.Thereby this attapulgite clay superparamagnetism matrix material can be handled under more low intensive electromagnetic field effect, adds manipulations such as can carrying out magnetic flocculation precipitate and separate, magnetic separation separation, magnetic filtration, target control under the electromagnetic field effect outside.Can be widely used in industrial raw material, comprise the fields such as purification, purifying air depth type filtration, nanofiltration membrane material, air quality surveillance filter material, coated material, water treatment and medical field targeted drug sustained release of gas and liquid.
Description of drawings:
Fig. 1 is equipped with magnetic granule-attapulgite composite material I process flow for the present invention with divalent iron salt nitrate oxidation direct crystallization legal system.
Fig. 2 is equipped with magnetic granule-attapulgite composite material I process flow for the present invention with divalent iron salt and trivalent iron salt direct crystallization legal system.
Fig. 3 is an images of transmissive electron microscope.According to the magnetic of embodiment 1 preparation-palygorskite nano composite material.The superparamagnetism iron oxide nanoparticles is in the distribution characteristics on attapulgite surface in the magnetic granule-attapulgite matrix material of demonstration direct crystallization method preparation, and maximum particle diameter is less than 30nm.
Fig. 4 is an images of transmissive electron microscope.According to the magnetic of embodiment 2 preparation-palygorskite nano composite material.Show that the superparamagnetism iron oxide nanoparticles is in the distribution characteristics on attapulgite surface in the magnetic granule-attapulgite matrix material, maximum particle diameter is less than 15nm.
Below the invention will be further described by embodiment:
Embodiment:
In following each embodiment, the attapulgite clay ore attapulgite content that is used for preparing the magnetic granule-attapulgite clay composite material is not less than 60%, quartzy and feldspar content is not higher than 5%, rhombspar content is not higher than 10%. attapulgite clays need not carry out drying treatment, directly push pugging and handle,, can add an amount of water if the ore water content is crossed when hanging down, satisfy the force into submission requirement of clay water content of extruding pugging, water content is controlled at 20%～60%.
Embodiment 1:
Concrete enforcement operated as follows:
1, to be made into mass volume ratio be 0.1: 100～20: 100 attapulgite clay suspension for the attapulgite clay that will handle through the extruding pugging and water, preferred solid-to-liquid ratio is 1: 100～5: 100, stirring impels the brilliant bundle of attapulgite to disperse, and forms stable attapulgite clay suspension;
2, under the powerful agitation condition, add divalent iron salt solution in the attapulgite clay suspension after dispersion treatment, the concentration of iron salt solutions is 1%～50%, and preferred concentration is 5%～10%.The mass ratio of iron and attapulgite clay is 100: 0.5～100: 30 in attapulgite clay and the molysite mixed solution, and preferred ratio is 100: 1～100: 5.The molysite of indication comprises ferrous sulfate, iron protochloride, iron trichloride.Above-mentioned suspension is heated to 50 ℃～100 ℃, and preferred value is 60 ℃～80 ℃ degree.
3, prepare nitrate and alkali lye mixing solutions in addition, the concentration of nitrate and alkali lye is 1%-20%, and preferred concentration is 5%-10%.Nitrate and alkali lye mixing solutions are heated to 50 ℃～100 ℃, and preferred value is 60 ℃～80 ℃.
4, the attapulgite-molysite mixed solution after the heating is mixed according to a certain percentage with nitrate-alkali lye mixed solution, the mol ratio that makes nitrate and molysite is 2: 1～1: 2, optimum ratio is 1: 1, and the mol ratio of alkali lye and molysite is 2: 1～4: 1, and optimum ratio is 3: 1; Mixed solution is heated to 50 ℃～100 ℃, stirs aging crystallization 0.5～5 hour.
5, the suspension dehydration, washing, the drying that step 4 are made obtain the magnetic granule-attapulgite clay composite material.Gained magnetic granule-attapulgite clay composite material susceptibility is greater than 1000SI (* 10
-8m
3/ kg), the particle diameter of magnetic-particle is less than 30 nanometers (as shown in Figure 3).
6, the magnetic granule-attapulgite clay composite material of step 5 gained was calcined 5 minutes to 2 hours at 200 ℃～400 ℃, obtained maghemite-attapulgite clay matrix material.
Embodiment 2:
Different is with the foregoing description 1, for the magnetic-particle crystal particle diameter that direct crystallization forms from solution is diminished, in the prepared attapulgite clay suspension of step 1, add citric acid or Citrate trianion or the phosphoric acid salt that accounts for attapulgite clay weight 0.1%, as the crystal growth control agent.Other each step is all identical with embodiment 1.The final magnetic-particle particle diameter that obtains to load on the attapulgite surface is in less than 15 nanometers (shown in Figure 4).
Embodiment 3:
Concrete enforcement operated as follows:
1, to be made into mass volume ratio be 0.1: 100～20: 100 attapulgite clay suspension for the attapulgite clay that will handle through the extruding pugging and water, preferred solid-to-liquid ratio is 1: 100～5: 100, stirring impels the brilliant bundle of attapulgite to disperse, and forms stable attapulgite clay suspension;
2, the mixing solutions that adds divalent iron salt and trivalent iron salt under the powerful agitation condition in the attapulgite clay suspension after dispersion treatment.The mol ratio of divalent iron salt and trivalent iron salt is 3: 1～1: 1, and preferred value is 1: 1;
3, add alkali lye under powerful the stirring in above-mentioned suspension, the mol ratio of alkali lye and molysite is 8: 3, stirs aging crystallization 0.5～5 hour.
4, the suspension dehydration, washing, the drying that above-mentioned steps are made obtain the magnetic granule-attapulgite clay composite material.Gained magnetic-palygorskite nano composite material susceptibility is greater than 1000SI (* 10
-8m
3/ kg), the particle diameter of magnetic-particle is less than 30 nanometers.
Embodiment 4:
Different is with the foregoing description 3, for the magnetic-particle crystal particle diameter that direct crystallization forms from solution is diminished, in the prepared attapulgite clay suspension of step 1, add citric acid or Citrate trianion or the phosphoric acid salt that accounts for attapulgite clay weight 0.1%, as the crystal growth control agent.Other each step is all identical with embodiment 3.
Gained magnetic-palygorskite nano composite material susceptibility is greater than 1000SI (* 10
-8m
3/ kg), the particle diameter of magnetic-particle is less than 15 nanometers.
In the above-described embodiments, nitrate is SODIUMNITRATE or saltpetre, and alkali lye is sodium hydroxide solution or potassium hydroxide solution or ammoniacal liquor or lime suspension, and molysite comprises ferrous sulfate, iron protochloride, iron trichloride.
Claims (4)
1. the preparation method of magnetic granule-attapulgite nano composite material, it is characterized in that with attapulgite clay and molysite be raw material, by attapulgite clay inductive divalence or divalence and ferric ion in attapulgite surface nucleation and attapulgite clay stabilization to nucleus, make directly crystallization from solution of nano magnetic particle, and load on the attapulgite plane of crystal, constitute supperparamagnetic particles-attapulgite matrix material; Described molysite is ferrous sulfate, iron protochloride or iron trichloride; Described method is carried out as follows:
A, attapulgite clay impel the brilliant Shu Xieju of attapulgite through the extruding pugging, being made into mass volume ratio with water is 0.1: 100～20: 100 attapulgite clay suspension, stirring impels the brilliant bundle of attapulgite to disperse, and forms stable attapulgite clay suspension;
B, operate by one of following dual mode:
Mode one: in the time of stirring, add divalent iron salt solution in the attapulgite clay suspension after dispersion treatment, iron salt solutions concentration is 1%～50%, and the mass ratio of iron and attapulgite clay is 100: 0.5～100: 30 in attapulgite clay and the molysite mixed solution; Attapulgite-molysite mixed solution is heated to 50 ℃～100 ℃; The nitrate solution and the alkali lye that are 1%-20% with concentration mix, and the preparation mixed solution is heated to 50～100 ℃ with the mixed solution of described nitrate solution and alkali lye; Described attapulgite-molysite mixed solution is mixed with nitrate-alkali lye mixed solution, and reheat to 50 ℃～100 ℃ stirs aging crystallization 0.5～5 hour; The mol ratio that the nitrate solution that is added and the amount of alkali lye are controlled at nitrate and molysite is 2: 1～1: 2, and the mol ratio of alkali lye and molysite is 2: 1～4: 1;
Mode two: in the time of stirring, add the mixing solutions of divalent iron salt and trivalent iron salt in the attapulgite clay suspension after dispersion treatment, the concentration of iron salt solutions is 1%～50%; The mol ratio of divalent iron salt and trivalent iron salt is 3: 1～1: 1; It is 0.001-0.1 that control molysite add-on makes iron in the suspension/attapulgite ratio; Under agitation condition, in attapulgite-molysite mixed solution, add alkali lye, the mol ratio of alkali lye and molysite is 4: 1-2: 1; Stir aging crystallization 0.5～5 hour;
Described nitrate is SODIUMNITRATE or saltpetre; Described alkali lye is sodium hydroxide solution or potassium hydroxide solution or ammoniacal liquor or lime suspension;
C, with suspension dehydration, washing, drying after the aging crystallization of step b, obtain magnetite-attapulgite clay matrix material.
2. preparation method according to claim 1 is characterized in that:
Among the described step a, attapulgite clay impels the brilliant Shu Xieju of attapulgite through the extruding pugging, and the mass volume ratio of the attapulgite clay suspension that is made into water is 1: 100～5: 100;
Mode one is when stirring among the described step b, the concentration of the divalent iron salt solution that adds in the attapulgite clay suspension after dispersion treatment is 5%～10%, and the mass ratio of iron and the withered soil of attapulgite is 100: 1～100: 5 in attapulgite clay and the molysite mixed solution; Attapulgite-molysite mixed solution is heated to 60 ℃～80 ℃; The nitrate solution and the alkali lye that are 5%-10% with concentration mix, and the preparation mixed solution is heated to 60 ℃～80 ℃ with the mixed solution of described nitrate solution and alkali lye; Described attapulgite-molysite mixed solution is mixed with nitrate-alkali lye mixed solution, and reheat to 50 ℃～100 ℃ stirs aging crystallization 0.5～5 hour; The mol ratio that the nitrate that is added and the amount of alkali lye are controlled at nitrate and molysite is 1: 1, and the mol ratio of alkali lye and molysite is 3: 1;
Mode two is when stirring among the described step b, and the divalent iron salt that adds in the attapulgite clay suspension after dispersion treatment and the mixing solutions concentration of trivalent iron salt are 5%～10%; The mol ratio of divalent iron salt and trivalent iron salt is 1: 1; It is 0.001-0.1 that control molysite add-on makes iron in the suspension/attapulgite ratio; Under agitation condition, in attapulgite-molysite mixed solution, add alkali lye, the mol ratio of alkali lye and molysite is 4: 1-2: 1; Stir aging crystallization 0.5～5 hour.
3. preparation method according to claim 1 and 2 is characterized in that add citric acid or Citrate trianion or the phosphoric acid salt that accounts for attapulgite clay weight 0.1% in the prepared attapulgite clay suspension of step a, as the crystal growth control agent.
4. preparation method according to claim 1 and 2 is characterized in that under normal pressure, 200 ℃～400 ℃ conditions step c gained magnetite-attapulgite clay matrix material being calcined 5 minutes to 2 hours, obtains maghemite-attapulgite clay matrix material.
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| CN101423273B (en) * | 2008-11-18 | 2010-08-25 | 江苏大学 | Composite paramagnetic nano flocculant and preparation method thereof |
| CN103086392B (en) * | 2011-11-03 | 2014-09-17 | 中国科学院兰州化学物理研究所 | Method for lengthening of short rod crystal attapulgite |
| CN102531157B (en) * | 2012-03-02 | 2014-08-06 | 合肥工业大学 | Biological aerated filter packing and preparation method thereof |
| CN102649954A (en) * | 2012-05-17 | 2012-08-29 | 兰州大学 | Immobilized enzyme for magnetic nanometer clay carrier and regenerating method thereof |
| CN103771431A (en) * | 2013-12-18 | 2014-05-07 | 核工业北京地质研究院 | Magnetization method of kaolinite particle surface |
| CN104086221B (en) * | 2014-07-12 | 2016-03-16 | 东北师范大学 | The preparation method of magnetic Bubbled stone carrier and the application in sewage disposal thereof |
| CN105601559B (en) * | 2014-12-02 | 2018-01-09 | 安徽星宇化工有限公司 | A kind of synthetic method of 2 pyridine carboxaldehyde |
| CN106268812A (en) * | 2016-08-25 | 2017-01-04 | 扬州大学 | A kind of nano-magnetic ecological restoration material on the ferroso-ferric oxide load attapulgite removing removal organic polluter and preparation method thereof |
| CN108236916A (en) * | 2016-12-27 | 2018-07-03 | 海门市源美美术图案设计有限公司 | A kind of magnetic halloysite composite material and its application |
| CN108822612A (en) * | 2018-05-31 | 2018-11-16 | 句容市东山纸品厂 | A kind of preparation method and application of water-based ink modifying agent |
| CN108795147A (en) * | 2018-05-31 | 2018-11-13 | 句容市东山纸品厂 | A method of improving water-based ink adhesive force |
| CN114950345A (en) * | 2022-04-29 | 2022-08-30 | 东南大学 | Sulfur-resistant and water-resistant volatile heavy metal vapor adsorbent and preparation method and application thereof |
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Assignee: Anhui Mingmei Minchem Co., Ltd. Assignor: Hefei University of Technology Contract record no.: 2011340000004 Denomination of invention: Method for preparing magnetic granule-attapulgite nano composite material Granted publication date: 20080820 License type: Exclusive License Open date: 20061025 Record date: 20110228 |
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