CN103289136A - Sodium alginate and rectorite nanometer composite material preparation method - Google Patents
Sodium alginate and rectorite nanometer composite material preparation method Download PDFInfo
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- CN103289136A CN103289136A CN2013102498712A CN201310249871A CN103289136A CN 103289136 A CN103289136 A CN 103289136A CN 2013102498712 A CN2013102498712 A CN 2013102498712A CN 201310249871 A CN201310249871 A CN 201310249871A CN 103289136 A CN103289136 A CN 103289136A
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- sodium alginate
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Abstract
The invention discloses a sodium alginate and rectorite nanometer composite material preparation method, which comprises the following steps: A10, preparing a sodium alginate and rectorite mixed solution, wherein a mass ratio of the sodium alginate to the rectorite is 1:0.1-4; A 20, preparing a calcium chloride solution with a concentration of 0.2-1 mol/L; A30, adopting a dropping pipette to drop the sodium alginate and rectorite mixed solution in the calcium chloride solution to form a spherical composite body system; and A40, freezing the spherical composite body system for 24 h, and soaking with ethanol to obtain the target sample, wherein ethanol is adopted to carry out replacement washing 3-4 times to remove ice water. According to the sodium alginate and rectorite nanometer composite material preparation method, the powder rectorite is reformed into the granular rectorite so as to improve absorption capacity and a recovery rate of the rectorite, and conveniently recycle.
Description
Technical field
The present invention relates to the preparation of matrix material, be specifically related to the preparation method of a kind of sodium alginate and rectorite nano composite material.
Background technology
Rectorite leng is a kind of clay of laminar silicate mineral, as a kind of novel environmental material, enjoys investigator's attention in recent years.After surfactant-modified, its interlamellar spacing strengthens, and the surface charge number increases, and can be adsorbed with organic pollutants effectively.At present, the research that the rectorite modified back of powder is used for wastewater treatment is more, and adopt the applied research of particulate state modification rectorite adsorbent processing waste water less.Although modified powder shape rectorite leng has adsorption effect and bigger loading capacity preferably, but in actual applications, because Powdered modification rectorite leng easy swelling behind the water logging bubble forms the mud of dispersion suspension, settling property is relatively poor, cause follow-up solid-liquid separation very difficult, so limited its application in actual waste water is handled.
Sodium alginate is the natural polysaccharide carbohydrate that extracts from sea-tangle, be similar to the glycosaminoglycan in the extracellular matrix, no subacute/reaction of chronic toxicity or carinogenicity, can be used as edible foodstuff additive, also can be used as timbering material and be used for medical usage, possess excellent biological compatibility, be widely used in products such as food, medicine, weaving, printing and dyeing, papermaking, daily-use chemical industry, as uses such as thickening material, emulsifying agent, stablizer, tackiness agent and sizing agents.
Summary of the invention
Technical problem to be solved by this invention is the mud that Powdered modification rectorite leng easy swelling behind the water logging bubble forms dispersion suspension, and settling property is relatively poor, causes follow-up solid-liquid separation very difficult, is difficult to the problem of using in actual waste water is handled.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention provides the preparation method of a kind of sodium alginate and rectorite nano composite material, may further comprise the steps: the mixing solutions of A10, configuration sodium alginate and rectorite leng, wherein the quality of the two is 1:0.1～4; A20, compound concentration are the calcium chloride solution of 0.2～1mol/L; A30, with minim pipette the mixing solutions of sodium alginate and rectorite leng is dropped in and to form spherical compound system in the calcium chloride solution; A40, will use alcohol immersion after the freezing 24h of spherical compound system, and change clothes deicing water 3～4 times with ethanol between soak period, finally obtain target sample.
In the preparation method of above-mentioned sodium alginate and rectorite nano composite material, in steps A 10, elder generation's water fully dissolves sodium alginate makes sodium alginate soln, the two mass ratio is 30:1, water fully dissolves rectorite leng and makes rectorite leng solution again, the two mass ratio is 10:1, keep in rectorite leng solution, slowly adding under the churned mechanically situation sodium alginate soln of getting ready, after mixing, restir 2h in 60 ℃ water bath with thermostatic control obtains mixing solutions and the cooling of sodium alginate and rectorite leng.
In the preparation method of above-mentioned sodium alginate and rectorite nano composite material, in steps A 30, spherical compound system is immersed in 2h in the calcium chloride solution.
In the preparation method of above-mentioned sodium alginate and rectorite nano composite material, in steps A 40, the freezing temp of spherical compound system is-10 ℃.
In the preparation method of above-mentioned sodium alginate and rectorite nano composite material, in steps A 40, the alcohol immersion time of spherical compound system is 24h.
The preparation method of sodium alginate provided by the invention and rectorite nano composite material transform pulverous rectorite leng as particulate state, improves adsorptive power and the rate of recovery of rectorite leng, conveniently recycles.
Description of drawings
Fig. 1 is the stereoscan photograph of embodiment 1;
Fig. 2 is the stereoscan photograph of embodiment 3.
Embodiment
At present, the research that the rectorite modified back of powder is used for wastewater treatment is more, and adopt the applied research of particulate state modification rectorite adsorbent processing waste water less.Therefore, we will be to rectorite modified, by method such as sodium alginate-modified, transform pulverous rectorite leng the particulate state of porous as, under the prerequisite that keeps original adsorptive power, improves the rate of recovery of rectorite leng, conveniently recycles.Develop a kind of environmental protection, composite porous preparation method easy and simple to handle, low-cost, high performance has important practical significance.
The preparation method of sodium alginate provided by the invention and rectorite nano composite material may further comprise the steps:
The mixing solutions of A10, configuration sodium alginate and rectorite leng, wherein the quality of the two is 1:0.1～4.Configuration flow is as follows: first water fully dissolves sodium alginate makes sodium alginate soln, the two mass ratio is 30:1, water fully dissolves rectorite leng and makes rectorite leng solution again, the two mass ratio is 10:1, keep in rectorite leng solution, slowly adding under the churned mechanically situation sodium alginate soln of getting ready, after mixing, restir 2h in 60 ℃ water bath with thermostatic control obtains mixing solutions and the cooling of sodium alginate and rectorite leng.
A20, compound concentration are the calcium chloride solution of 0.2～1mol/L.
A30, with minim pipette the mixing solutions of sodium alginate and rectorite leng is dropped in and to form spherical compound system in the calcium chloride solution, and spherical compound system is immersed in 2h in the calcium chloride solution;
A40, spherical compound system is down used alcohol immersion after the freezing 24h at-10 ℃, soak time is 24h, and changes clothes deicing water 3～4 times with ethanol between soak period, finally obtains target sample, is called B to be.
For steps A 40, also have another kind of contrast alternate process method, namely dry under 50 ℃-60 ℃, obtain control sample, be called A system.
Be further described below in conjunction with the present invention of embodiment, wherein the rectorite leng raw material is the sodium rectorite leng that is provided by Hubei distinguished personages' rectorite leng Science and Technology Ltd..
Embodiment 1(Comparative Examples):
In the ratio of sodium alginate and rectorite leng mass ratio 1:2, mix obtaining dispersed system, in 60 ℃ water bath with thermostatic control, stir 2h; Cooling splashes into glomeration in the calcium chloride solution (concentration is 0.5mol/L) with compound system, is immersed in about 2h in the calcium chloride solution; Dry under 50 ℃-60 ℃, obtain sample.
Embodiment 2(Comparative Examples):
In the ratio of sodium alginate and rectorite leng mass ratio 1:1, mix obtaining dispersed system, in 60 ℃ water bath with thermostatic control, stir 2h; Cooling splashes into glomeration in the calcium chloride solution (concentration is 0.2mol/L) with compound system, is immersed in about 2h in the calcium chloride solution; Dry under 50 ℃, obtain sample.
Embodiment 3:
In the ratio of sodium alginate and rectorite leng mass ratio 1:2, mix obtaining dispersed system, in 60 ℃ water bath with thermostatic control, stir 2h; Cooling splashes into glomeration in the calcium chloride solution (concentration is 0.5mol/L) with compound system, is immersed in about 2h in the calcium chloride solution; Use alcohol immersion after-10 ℃ of freezing 24h, during change clothes 3 deicing (water) with ethanol, obtain sample.
Embodiment 4:
In the ratio of sodium alginate and rectorite leng mass ratio 1:1, mix obtaining dispersed system, in 60 ℃ water bath with thermostatic control, stir 2h; Cooling splashes into glomeration in the calcium chloride solution (concentration is 0.2mol/L) with compound system, is immersed in about 2h in the calcium chloride solution; Use alcohol immersion after-10 ℃ of freezing 24h, during change clothes 3 deicing (water) with ethanol, obtain sample.
Embodiment 5:
In the ratio of sodium alginate and rectorite leng mass ratio 1:4, mix obtaining dispersed system, in 60 ℃ water bath with thermostatic control, stir 2h; Cooling splashes into glomeration in the calcium chloride solution (concentration is 1mol/L) with compound system, is immersed in about 2h in the calcium chloride solution; Use alcohol immersion after-15 ℃ of freezing 24h, during change clothes 3 deicing (water) with ethanol, obtain sample.
The sample that adopts above-described embodiment to obtain is tested:
(1) scanning electron microscope analysis:
Utilize scanning electron microscope to carry out microscopic appearance and observe, the instrument of employing is Philips XL-3 type environmental scanning electron microscope, observes the cross section pattern under Electronic Speculum, as shown in Figure 1 and Figure 2.
(2) absorption property test:
Adopt spectrophotometry to determine methylene blue concentration by measuring the methylene blue solution absorbancy.Prepare the methylene blue solution of different concns respectively and measure each solution absorbency at the 662nm place with spectrophotometer, carry out linear regression and get typical curve.
In the water bath with thermostatic control vibrator, adsorb 10mL(0.1mol/L with the 0.01g sorbent material) experiment of methylene blue solution, measure the methylene blue solution absorbancy at set intervals respectively after the reaction beginning, draw the adsorptive capacity change with time of sample under a certain temperature according to typical curve, when absorbancy does not change in time, calculate equilibrium adsorption capacity according to absorbancy.Following table is the embodiment sample to the equilibrium adsorption capacity of methylene blue dye:
| Embodiment | Equilibrium adsorption capacity (mg/g, dyestuff/sorbent material) |
| Sodium alginate | 2.35 |
| Rectorite leng | 32.5 |
| 1(A system) | 7.51 |
| 2(A system) | 6.06 |
| 3(B system) | 32.3 |
| 4(B system) | 22.4 |
| 5(B system) | 30.5 |
Beneficial effect of the present invention is as follows:
(1) sodium alginate derives from natural phant, and rectorite leng derives from natural mineral, and low price is nontoxic material.Hydrophilic radical on the rectorite leng can form good interaction of hydrogen bond with the hydroxyl of Lalgine, transform pulverous rectorite leng as particulate state, improves adsorptive power and the rate of recovery of rectorite leng, conveniently recycles.
(2) after the sodium alginate after the modification-rectorite leng matrix material is handled through freezing-exchange of solvent, obtain sample B system, the adsorptive power more not A based material of freezing treatment has remarkable lifting.Because refrigerating process is slow, can fully form ice crystal, makes structure fluffy, form vesicular structure, surface-area increases, thereby promotes adsorptive power.
The present invention is not limited to above-mentioned preferred forms, and anyone should learn the structural changes of making under enlightenment of the present invention, and every have identical or close technical scheme with the present invention, all falls within protection scope of the present invention.
Claims (5)
1. the preparation method of sodium alginate and rectorite nano composite material is characterized in that, may further comprise the steps:
The mixing solutions of A10, configuration sodium alginate and rectorite leng, wherein the quality of the two is 1:0.1～4;
A20, compound concentration are the calcium chloride solution of 0.2～1mol/L;
A30, with minim pipette the mixing solutions of sodium alginate and rectorite leng is dropped in and to form spherical compound system in the calcium chloride solution;
A40, will use alcohol immersion after the freezing 24h of spherical compound system, and change clothes deicing water 3～4 times with ethanol between soak period, finally obtain target sample.
2. the preparation method of sodium alginate as claimed in claim 1 and rectorite nano composite material, it is characterized in that, in steps A 10, elder generation's water fully dissolves sodium alginate makes sodium alginate soln, the two mass ratio is 30:1, water fully dissolves rectorite leng and makes rectorite leng solution again, the two mass ratio is 10:1, keep in rectorite leng solution, slowly adding under the churned mechanically situation sodium alginate soln of getting ready, after mixing, restir 2h in 60 ℃ water bath with thermostatic control obtains mixing solutions and the cooling of sodium alginate and rectorite leng.
3. the preparation method of sodium alginate as claimed in claim 1 and rectorite nano composite material is characterized in that, in steps A 30, spherical compound system is immersed in 2h in the calcium chloride solution.
4. the preparation method of sodium alginate as claimed in claim 1 and rectorite nano composite material is characterized in that, in steps A 40, the freezing temp of spherical compound system is-10 ℃.
5. the preparation method of sodium alginate as claimed in claim 1 and rectorite nano composite material is characterized in that, in steps A 40, the alcohol immersion time of spherical compound system is 24h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107043493A (en) * | 2017-04-07 | 2017-08-15 | 安徽省无为县经纬电缆附件有限公司 | A kind of heating cable protective cover material of good heat preservation performance |
| CN113000037A (en) * | 2021-04-12 | 2021-06-22 | 中国科学院南京土壤研究所 | Composite microsphere adsorbent for treating ammonia nitrogen and heavy metal composite polluted wastewater in rare earth mining area and preparation method and application thereof |
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| CN101810863A (en) * | 2009-12-17 | 2010-08-25 | 华南理工大学 | Preparation method of carboxymethyl chitosan quaternary ammonium salt/organic rectorite nano composite material and application thereof |
| CN102302924A (en) * | 2011-08-18 | 2012-01-04 | 江苏科技大学 | Preparation method of microsphere adsorbent based on rectorite |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101810863A (en) * | 2009-12-17 | 2010-08-25 | 华南理工大学 | Preparation method of carboxymethyl chitosan quaternary ammonium salt/organic rectorite nano composite material and application thereof |
| CN102302924A (en) * | 2011-08-18 | 2012-01-04 | 江苏科技大学 | Preparation method of microsphere adsorbent based on rectorite |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107043493A (en) * | 2017-04-07 | 2017-08-15 | 安徽省无为县经纬电缆附件有限公司 | A kind of heating cable protective cover material of good heat preservation performance |
| CN113000037A (en) * | 2021-04-12 | 2021-06-22 | 中国科学院南京土壤研究所 | Composite microsphere adsorbent for treating ammonia nitrogen and heavy metal composite polluted wastewater in rare earth mining area and preparation method and application thereof |
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