CN110975834A - Ultra-light floatable material and preparation method and application thereof - Google Patents

Ultra-light floatable material and preparation method and application thereof Download PDF

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CN110975834A
CN110975834A CN201911317353.3A CN201911317353A CN110975834A CN 110975834 A CN110975834 A CN 110975834A CN 201911317353 A CN201911317353 A CN 201911317353A CN 110975834 A CN110975834 A CN 110975834A
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sodium alginate
ultra
floatable material
light
oil
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CN110975834B (en
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高云玲
孙晓斐
贠军贤
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Zhejiang University of Technology ZJUT
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Zhejiang University of Technology ZJUT
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    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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Abstract

The invention discloses an ultralight floatable material, a preparation method and application thereof, and the preparation method of the ultralight floatable material comprises the following steps: 1) uniformly mixing a sodium alginate solution, calcium carbonate and gluconic acid-delta-lactone, and freeze-drying to obtain sodium alginate-based aerogel; 2) soaking the sodium alginate-based aerogel obtained in the step 1) in a metal salt solution, adding hydrazine hydrate, washing the aerogel with water after soaking, and freeze-drying to obtain the ultralight floatable material. The ultralight floatable material prepared by the technical scheme of the invention has the characteristics of simple and quick method, can float on the water surface, has good absorption effect, is used for treating oily sewage or sewage containing a nonpolar organic solvent, and has the characteristics of high efficiency and environmental protection.

Description

Ultra-light floatable material and preparation method and application thereof
Technical Field
The invention relates to the technical field of chemical materials, in particular to an ultra-light floatable material and a preparation method and application thereof.
Background
The demand of technological development for oil is more and more extensive, and the oil leakage and discharge caused by the activities of oil exploitation, transportation, offshore storage and the like also cause marine pollution and the generation of oily wastewater. Industrially, production of various agricultural chemicals, etc. also uses a large amount of nonpolar organic solvent, eventually causing accumulation of nonpolar organic solvent waste water. Wastewater containing oil or nonpolar organic solvent is characterized by complex components and great treatment difficulty.
The treatment method of the wastewater containing oil or non-polar organic solvent comprises gravity separation, physical adsorption, electrochemical treatment, biological treatment and the like, and has the problems of insufficient treatment capacity, low separation efficiency and secondary pollution, so that the search for a high-efficiency and oil-absorbing material is urgent.
The sodium alginate is derived from natural algae, has good biocompatibility and easily obtained raw materials. Sodium alginate is used as a substrate of the material, a three-dimensional space hydrogel is formed by adding a cross-linking agent, and the material which is ultra-light and can float on the water surface is obtained by freezing and nano-particle formation, so that the direct removal of oily sewage becomes possible.
Disclosure of Invention
In view of the problems in the prior art, the invention aims to provide an ultra-light floatable material, a preparation method and application thereof, and the ultra-light floatable material has the characteristics of simple preparation method, capability of efficiently treating sewage containing oil or non-polar organic solvents, environmental friendliness.
The preparation method of the ultralight floatable material is characterized by comprising the following steps:
1) uniformly mixing a sodium alginate solution, calcium carbonate and gluconic acid-delta-lactone, and freeze-drying to obtain sodium alginate-based aerogel;
2) soaking the sodium alginate-based aerogel obtained in the step 1) in a metal salt solution, adding hydrazine hydrate, washing the aerogel with water after soaking, and freeze-drying to obtain the ultralight floatable material.
The preparation method of the ultralight floatable material is characterized in that the specific process of the step 1) is as follows: adding calcium carbonate powder into a sodium alginate solution, uniformly stirring to obtain a suspension solution, adding gluconic acid-delta-lactone powder into the suspension solution, uniformly stirring, standing, pre-freezing in a refrigerator, and quickly transferring to a freeze dryer for drying after pre-freezing to obtain the sodium alginate-based hydrogel.
The preparation method of the ultralight floatable material is characterized in that in the step 1), the concentration of sodium alginate is 0.5-5wt%, and the mass ratio of sodium alginate to calcium carbonate is 1:10-1: 20.
The preparation method of the ultralight floatable material is characterized in that in the step 1), the molar ratio of calcium carbonate to gluconic acid-delta-lactone is 1:1-3: 1.
The preparation method of the ultralight floatable material is characterized in that in the step 2), reactants are washed by water and then put into a refrigerator for pre-freezing, and the reactants are quickly transferred into a freeze dryer for drying after being pre-frozen, so that the ultralight floatable material is obtained.
The preparation method of the ultralight floatable material is characterized in that in the step 2), the mass ratio of sodium alginate to metal salt is 1:0.1-1:1.9, and the metal salt is silver salt and copper salt, preferably silver nitrate or copper acetate.
The preparation method of the ultralight floatable material is characterized in that in the step 2), the molar ratio of the metal salt to the hydrazine hydrate is 1:10-1: 32.
The ultra-light floatable material obtained by the preparation method can float on the surface of seawater or fresh water.
The ultra-light floatable material is used as an adsorbent and is characterized by being used for adsorbing oil or an organic solvent, wherein the oil is offshore spilled oil, organic rapeseed oil, vacuum pump oil or methyl silicone oil, and the organic solvent is a nonpolar organic solvent.
The use is characterized in that the absorption capacity for oils or organic solvents is 4.2 to 9.7 g/g.
Compared with the prior art, the invention has the beneficial effects that:
the ultralight floatable material obtained by the limited preparation method disclosed by the invention takes sodium alginate as a matrix, is good in biocompatibility, easy to obtain, free of secondary pollution and low in density, can float on the water surface, is simple and rapid in preparation method, can be produced in a large scale, can be used for efficiently treating oily sewage or sewage containing non-polar organic solution, and is green and environment-friendly.
Drawings
Fig. 1 is a diagram illustrating a floating state of an ultra-light floatable material prepared in example 6 of the present invention on a water surface;
fig. 2 is a graph showing the effect of the ultra-light floatable material prepared in example 6 of the present invention on the adsorption of oil and solvent.
Detailed Description
The invention is further described with reference to specific examples, but the scope of protection of the invention is not limited to the described ranges.
Example 1
Adding 0.183g of calcium carbonate powder into 100ml of sodium alginate solution with the mass fraction of 1%, stirring uniformly, then adding 0.6514g of gluconic acid-delta-lactone powder into the suspension, stirring uniformly for 5min, standing the mixture for 48h, placing the mixture into a refrigerator for pre-freezing, quickly transferring the mixture into a freeze dryer for drying after pre-freezing for 4h, and obtaining 1% sodium alginate-based aerogel; the prepared aerogel material is soaked in 1mmol of silver nitrate water solution, 1.0mL of hydrazine hydrate (mass fraction is 85%) is added, after 12 hours of reaction, the obtained material is washed by water, and finally the material is pre-frozen in a refrigerator for 4 hours and then is quickly transferred to a freeze dryer for drying, so that the ultra-light floatable material is obtained, and the absorption capacity of the material to rapeseed oil at room temperature is 5.74 g/g.
Example 2
Adding 0.366g of calcium carbonate powder into 100mL of sodium alginate solution with the mass fraction of 2%, stirring uniformly, adding 1.3028g of gluconic acid-delta-lactone powder into the suspension, stirring uniformly for 5min, standing the mixture for 48h, placing the mixture into a refrigerator for prefreezing, quickly transferring the mixture into a freeze dryer for drying after prefreezing for 4h to obtain 2% sodium alginate-based aerogel, soaking the prepared aerogel material into 1mmol of silver nitrate aqueous solution, adding 1.0mL of hydrazine hydrate (with the mass fraction of 85%), reacting for 12h, washing the obtained material with water, quickly transferring the material into the freeze dryer for drying after prefreezing for 4h in the refrigerator to obtain the ultra-light floatable material, wherein the absorption capacity of the material to rapeseed oil at room temperature is 5.05 g/g.
Example 3
Adding 0.549g of calcium carbonate powder into 100mL of sodium alginate solution with the mass fraction of 3%, stirring uniformly, adding 1.9542g of gluconic acid-delta-lactone powder into the suspension, stirring uniformly for 5min, standing the mixture for 48h, placing the mixture into a refrigerator for prefreezing, quickly transferring the mixture into a freeze dryer for drying after prefreezing for 4h to obtain 3% sodium alginate-based aerogel, soaking the prepared aerogel material into 5mmol of silver nitrate aqueous solution, adding 5.0mL of hydrazine hydrate (with the mass fraction of 85%), reacting for 12h, washing the obtained material with water, quickly transferring the material into the freeze dryer for drying after prefreezing for 4h in the refrigerator to obtain the ultra-light floatable material, wherein the absorption capacity of the material to the rapeseed oil at room temperature is 2.99 g/g.
Example 4
Adding 0.366g of calcium carbonate powder into 100mL of sodium alginate solution with the mass fraction of 2%, stirring uniformly, adding 1.3028g of gluconic acid-delta-lactone powder into the suspension, stirring uniformly for 5min, standing the mixture for 48h, placing the mixture into a refrigerator for prefreezing, quickly transferring the mixture into a freeze dryer for drying after prefreezing for 4h to obtain 2% sodium alginate-based aerogel, soaking the prepared aerogel material into 2mmol of copper acetate aqueous solution, adding 2.0mL of hydrazine hydrate (with the mass fraction of 85%), reacting for 12h, washing the obtained material with water, quickly transferring the material into the freeze dryer for drying after prefreezing for 4h in the refrigerator to obtain the ultra-light floatable material, wherein the absorption capacity of the material to rapeseed oil at room temperature is 3.62 g/g.
Example 5
Adding 0.183g of calcium carbonate powder into 100mL of sodium alginate solution with the mass fraction of 1%, stirring uniformly, adding 0.6514g of gluconic acid-delta-lactone powder into the suspension, stirring uniformly for 5min, standing the mixture for 48h, placing the mixture into a refrigerator for prefreezing, quickly transferring the mixture into a freeze dryer for drying after prefreezing for 4h to obtain 1% sodium alginate-based aerogel, soaking the prepared aerogel material into 1mmol of copper acetate aqueous solution, adding 1.0mL of hydrazine hydrate (with the mass fraction of 85%), reacting for 12h, washing the obtained material with water, quickly transferring the material into the freeze dryer for drying after prefreezing for 4h in the refrigerator to obtain the ultra-light floatable material, wherein the absorption capacity of the material to rapeseed oil at room temperature is 4.97 g/g.
Example 6
Adding 0.366g of calcium carbonate powder into 100mL of sodium alginate solution with the mass fraction of 2%, stirring uniformly, adding 1.3028g of gluconic acid-delta-lactone powder into the suspension, stirring uniformly for 5min, standing the mixture for 48h, placing the mixture into a refrigerator for prefreezing, quickly transferring the mixture into a freeze dryer for drying after prefreezing for 4h to obtain 2% sodium alginate-based aerogel, soaking the prepared aerogel material into 1mmol of copper acetate aqueous solution, adding 1.0mL of hydrazine hydrate (with the mass fraction of 85%), reacting for 12h, washing the obtained material with water, quickly transferring the material into the freeze dryer for drying after prefreezing for 4h in the refrigerator to obtain the ultra-light floatable material, wherein the absorption capacity of the material to rapeseed oil at room temperature is 4.29 g/g.
Example 7
Aerogel material prepared in example 6 (1 cm. times.1 cm) was first weighed and the mass recorded as m0Soaking aerogel in various oils or organic solvents (such as rapeseed oil, vacuum pump oil, chloroform, n-hexane, etc.) at room temperature, taking out after adsorption reaches equilibrium for a period of time, slightly wiping the surface with a piece of filter paper within 5 s to remove excessive oil or solvent, and rapidly weighing to obtain a mass m1The oil absorption was calculated according to the following formula:
oil absorption (g/g) = (m)1-m0)/m0，
As shown in fig. 1, the ultra-light floatable material prepared in example 6 floats on the water surface; as can be seen from FIG. 2, the ultra-light floatable material prepared in example 6 has an absorption capacity of 4.2 to 9.7g/g for oil or solvent at room temperature.

Claims (10)

1. A preparation method of an ultralight floatable material is characterized by comprising the following steps:
1) uniformly mixing a sodium alginate solution, calcium carbonate and gluconic acid-delta-lactone, and freeze-drying to obtain sodium alginate-based aerogel;
2) soaking the sodium alginate-based aerogel obtained in the step 1) in a metal salt solution, adding hydrazine hydrate, washing the aerogel with water after soaking, and freeze-drying to obtain the ultralight floatable material.
2. The method for preparing the ultra-light floatable material according to claim 1, wherein the specific process of the step 1) is as follows: adding calcium carbonate powder into a sodium alginate solution, uniformly stirring to obtain a suspension solution, adding gluconic acid-delta-lactone powder into the suspension solution, uniformly stirring, standing, pre-freezing in a refrigerator, and quickly transferring to a freeze dryer for drying after pre-freezing to obtain the sodium alginate-based hydrogel.
3. The method for preparing an ultra-light floatable material according to claim 1 or 2, characterized in that in step 1), the concentration of sodium alginate is 0.5-5wt%, and the mass ratio of sodium alginate to calcium carbonate is 1:10-1: 20.
4. The method for preparing an ultra-light floatable material according to claim 1 or 2, characterized in that in step 1), the molar ratio of calcium carbonate to glucono-delta-lactone is 1:1 to 3: 1.
5. The method for preparing an ultra-light floatable material according to claim 1, wherein in the step 2), the reactant is washed with water and then put into a refrigerator for pre-freezing, and after pre-freezing, the reactant is rapidly transferred to a freeze dryer for drying to obtain the ultra-light floatable material.
6. The method for preparing an ultra-light floatable material according to claim 1 or 5, characterized in that in step 2), the mass ratio of sodium alginate to metal salt is 1:0.1-1:1.9, and the metal salt is silver salt and copper salt, preferably silver nitrate or copper acetate.
7. The method for preparing an ultra-light floatable material according to claim 1, wherein in the step 2), the molar ratio of the metal salt to the hydrazine hydrate is 1:10 to 1: 32.
8. An ultra-light floatable material obtained by the preparation method according to claim 1, which is floatable on seawater or fresh water.
9. Use of the ultra-light floatable material according to claim 8 as an adsorbent for adsorbing oil or organic solvents, wherein the oil is marine spill oil, rapeseed oil, vacuum pump oil or methyl silicone oil and the organic solvent is a non-polar organic solvent.
10. Use according to claim 9, characterized in that the absorption capacity for oils or organic solvents is between 4.2 and 9.7 g/g.
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CN108160051A (en) * 2018-01-18 2018-06-15 南京工业大学 A kind of preparation method of calcium alginate aerogel material
CN108178152A (en) * 2018-03-01 2018-06-19 济南开发区星火科学技术研究院 It is a kind of can efficient absorption heavy metal ion graphite oxide aerogel preparation method
CN108816291A (en) * 2018-05-14 2018-11-16 福建农林大学 A kind of alginic acid alkali composite photocatalyst aerogel material and preparation method thereof
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