CN114225914A - Preparation method of super-hydrophobic rod-shaped straw-based adsorption material - Google Patents
Preparation method of super-hydrophobic rod-shaped straw-based adsorption material Download PDFInfo
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- CN114225914A CN114225914A CN202111544932.9A CN202111544932A CN114225914A CN 114225914 A CN114225914 A CN 114225914A CN 202111544932 A CN202111544932 A CN 202111544932A CN 114225914 A CN114225914 A CN 114225914A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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Abstract
The invention discloses a preparation method of a super-hydrophobic rod-shaped straw-based adsorbing material. Selecting mature straw agricultural wastes, cutting the agricultural wastes into rod-shaped straws, and cleaning and drying the rod-shaped straws by using water; putting the rod-shaped straws into a glass dryer filled with a hydrophobic reagent, and standing at normal temperature; and then putting the mixture into a vacuum drying oven to prepare the product. According to the invention, the super-hydrophobic rod-shaped straw-based adsorption material is efficiently prepared by using super-hydrophobic treatment of one-step chemical vapor deposition, the hydrophobic angle is up to 161 degrees, the saturated adsorption capacity can be reached only within 20s, the high organic pollutant absorption rate is shown, the cyclic regeneration can be easily realized, and the resource utilization rate of agricultural wastes is improved.
Description
Technical Field
The invention relates to a preparation method of an adsorbing material in the field of resource utilization of agricultural wastes and removal of toxic and harmful environmental pollutants, and particularly relates to a preparation method of a super-hydrophobic rod-shaped straw-based adsorbing material.
Background
In the field of removing toxic and harmful environmental pollutants, the utilization of straw agricultural wastes is generally crushed, screened and then recycled. This makes the fine granular (or powdered) straw powder difficult to recycle after removing or catalytically degrading pollutants by adsorption, increases the use cost and has the risk of secondary environmental pollution.
The hydrophilic and oleophilic amphipathic property of the straws is not beneficial to exclusively removing hydrophobic organic pollutants in the environment, and limits the application range of the straws in the field of removing toxic and harmful organic pollutants. Hydrophobic strategies with different principles have been used for hydrophobic modification of powdery straws, and hydrophobic modification of rod-shaped straws has not been reported yet. The existing hydrophobic modification method usually needs to use a plurality of organic reagents or generate nano materials in situ at the same time, and has the disadvantages of complex operation and high cost.
The application of the straw agricultural wastes in the field of removing toxic and harmful environmental pollutants is greatly limited by the problems. Therefore, the development of a rod-shaped straw-based adsorption material which has super-hydrophobicity and can be recycled is urgently needed.
Disclosure of Invention
In order to solve the problems, the technical scheme of the invention is that rod-shaped straws are directly selected, and a one-step chemical vapor deposition method is utilized to provide a preparation method of a super-hydrophobic rod-shaped straw-based adsorption material.
Specifically, the technical scheme of the invention is as follows:
(1) selecting mature straw agricultural wastes, cutting the agricultural wastes into rod-shaped straws, cleaning the rod-shaped straws with water, and drying the rod-shaped straws for later use;
(2) putting the rodlike straws obtained in the step (1) into a brown glass dryer (the inner diameter of the brown glass dryer is 30cm) filled with a hydrophobic reagent, and reacting and standing for 12 hours under a normal temperature environment to obtain super-hydrophobic rodlike straws;
(3) and (3) putting the super-hydrophobic rod-shaped straw obtained in the step (2) into a vacuum drying box, and removing redundant hydrophobic reagents to obtain the super-hydrophobic rod-shaped straw-based adsorbing material.
The straw agricultural waste comprises cotton straw, corn straw, rape straw and the like. The straw agricultural waste is not only limited to cotton straw, but also is applicable to other mature crop straws, such as corn straw, rape straw and the like.
The length of the cut rodlike straw is 0.1-10 cm. Preferably 1cm in length.
The relative humidity in the brown glass dryer is controlled to be 15-85%.
The hydrophobic reagent is methyltrichlorosilane, an organosilane based hydrophobic reagent, or other organic reagent suitable for use in constructing a chemical vapor deposition process. The hydrophobic reagent is not limited to methyltrichlorosilane, but other organosilane based hydrophobic reagents or other organic reagents suitable for use in constructing a chemical vapor deposition process can be used.
The volume of the methyltrichlorosilane is 100-1000 mu L. The preferred volume of methyltrichlorosilane is 400. mu.L.
According to the invention, abundant hydroxyl groups contained in the rodlike straw and methyl trichlorosilane are subjected to a series of derivatization reactions, and a super-hydrophobic silane coating is generated on the surface of the straw, so that the super-hydrophobic rodlike straw-based adsorbing material is obtained.
The method specifically implements the method by taking the rodlike cotton straw as an example, directly selecting mature cotton straw as a base material, and utilizing a super-hydrophobic strategy of one-step chemical vapor deposition to efficiently prepare the super-hydrophobic rodlike cotton straw-based adsorbing material, wherein the hydrophobic angle can reach 161 degrees. Through tests, the material can reach adsorption saturation in only 20s, shows a faster organic pollutant absorption rate, and is far superior to other hydrophobic adsorption materials of the same type.
As shown in figure 4, the material can be recycled for at least more than 10 times through cleaning by chemical agents. The result shows that the material can be easily recycled, and the resource utilization rate of agricultural wastes is improved.
The invention has the beneficial effects that:
(1) and (4) performing one-step super-hydrophobic treatment. The chemical vapor deposition method is utilized, the super-hydrophobic property of the straw surface can be realized in one step, the preparation process is simple, the speed and the efficiency are high, the hydrophobic effect is good, and the cost is low.
(2) The dirt absorption speed is high. The absorption saturation can be completed only 20s by relying on the capillary action induced by the natural serial-through pit structure of the rod-shaped cotton straw and combining with the surface hydrophobic reinforcement as shown in figure 3, and the rate of absorbing organic pollutants is obviously superior to that of fine powder straw or other similar absorbing materials.
(3) And (5) simple regeneration. As shown in figure 4, after the rod-shaped cotton straws absorb organic pollutants, the rod-shaped cotton straws can be circularly regenerated by cleaning with chemical reagents, so that the resource utilization value of agricultural wastes is improved.
Drawings
FIG. 1 is a photograph showing the absorption of water and cyclohexane by cotton stalk in stick form before (a) and after (b) hydrophobic modification.
FIG. 2 is a photograph of water contact angle of the bar-shaped cotton stalk after hydrophobic modification.
FIG. 3 is a kinetic curve diagram of cyclohexane absorption of the cotton stalk after hydrophobic modification.
FIG. 4 is a diagram showing the recycling of the bar-shaped cotton stalks after hydrophobic modification.
Detailed Description
The advantages of the present invention can be further understood by the following detailed description in conjunction with the accompanying drawings.
Example 1
Selecting mature cotton straws, cutting the cotton straws into rod-shaped cotton straws with the length of 1cm, washing the cotton straws with water, and drying the cotton straws at 80 ℃. Putting the obtained rod-shaped cotton straw into a brown glass dryer with 400 mu L of methyltrichlorosilane and the internal diameter of 30cm, controlling the relative humidity in the brown glass dryer at 35%, and standing for 12h in a normal temperature environment. And then putting the hydrophobically modified rod-shaped cotton straw into a vacuum drying oven (80 ℃, 4h) to obtain the super-hydrophobic rod-shaped cotton straw-based adsorbing material.
The effect of absorbing water and cyclohexane before and after the hydrophobic modification of the example is shown in fig. 1, and it can be seen that the rod-shaped straw-based adsorbing material shows excellent hydrophobic effect after the hydrophobic modification. The material can only adsorb the organic pollutant cyclohexane and extremely repel water.
The result of the water contact angle test after the hydrophobic modification of this example is shown in fig. 2, and the water contact angle is 161 °. In the embodiment, through a dynamics test of the straw-based adsorption material, the test result is shown in fig. 3, and it can be seen that the material can reach adsorption saturation only in 20 s.
In the embodiment, the test result of the cyclic regeneration test of the straw-based adsorbing material is shown in fig. 4. As can be seen, the material can be recycled for at least more than 10 times, and shows excellent cyclic regeneration capacity.
Example 2
Selecting mature cotton straws, cutting the cotton straws into rod-shaped cotton straws with the length of 2cm, washing the cotton straws with water, and drying the cotton straws at 80 ℃. Putting the obtained rod-shaped cotton straw into a brown glass dryer with 400 mu L of methyltrichlorosilane and the internal diameter of 30cm, controlling the relative humidity in the brown glass dryer at 35%, and standing for 12h in a normal temperature environment. And then putting the hydrophobically modified rod-shaped cotton straw into a vacuum drying oven (80 ℃, 4h) to obtain the super-hydrophobic rod-shaped cotton straw-based adsorbing material.
Example 3
Selecting mature cotton straws, cutting the cotton straws into rod-shaped cotton straws with the length of 1cm, washing the cotton straws with water, and drying the cotton straws at 80 ℃. Putting the obtained rod-shaped cotton straw into a brown glass dryer with 600 mu L of methyltrichlorosilane and the internal diameter of 30cm, controlling the relative humidity in the brown glass dryer at 35%, and standing for 12h in a normal temperature environment. And then putting the hydrophobically modified rod-shaped cotton straw into a vacuum drying oven (80 ℃, 4h) to obtain the super-hydrophobic rod-shaped cotton straw-based adsorbing material.
Example 4
Selecting mature cotton straws, cutting the cotton straws into rod-shaped cotton straws with the length of 1cm, washing the cotton straws with water, and drying the cotton straws at 80 ℃. Putting the obtained rod-shaped cotton straw into a brown glass dryer with 600 mu L of methyltrichlorosilane and the internal diameter of 30cm, controlling the relative humidity in the brown glass dryer at 50%, and standing for 12h in a normal temperature environment. And then putting the hydrophobically modified rod-shaped cotton straw into a vacuum drying oven (80 ℃, 4h) to obtain the super-hydrophobic rod-shaped cotton straw-based adsorbing material.
Claims (6)
1. A preparation method of a super-hydrophobic rod-shaped straw-based adsorption material is characterized by comprising the following preparation steps:
(1) selecting mature straw agricultural wastes, cutting the agricultural wastes into rod-shaped straws, washing the rod-shaped straws with water and drying the rod-shaped straws;
(2) putting the rod-shaped straws obtained in the step (1) into a glass dryer filled with a hydrophobic reagent, and reacting and standing for 12 hours under a normal temperature environment to obtain super-hydrophobic rod-shaped straws;
(3) and (3) putting the super-hydrophobic rod-shaped straw obtained in the step (2) into a vacuum drying box, and removing redundant hydrophobic reagents to obtain the super-hydrophobic rod-shaped straw-based adsorbing material.
2. The preparation method of the super-hydrophobic rod-shaped straw-based adsorption material as claimed in claim 1, wherein the straw agricultural waste comprises cotton straw, corn straw, rape straw and the like.
3. The preparation method of the super-hydrophobic rod-shaped straw-based adsorbing material as claimed in claim 1, wherein the length of the rod-shaped straw after being cut is 0.1-10 cm.
4. The preparation method of the super-hydrophobic rod-like straw-based adsorbing material as claimed in claim 1, wherein the relative humidity in the glass dryer is controlled to be 15-85%.
5. The preparation method of the super-hydrophobic rod-shaped straw-based adsorption material as claimed in claim 1, wherein the hydrophobic reagent is methyltrichlorosilane, an organosilane hydrophobic reagent or other organic reagents suitable for construction of chemical vapor deposition.
6. The preparation method of the super-hydrophobic rod-like straw-based adsorbing material as claimed in claim 1, wherein the volume of the methyltrichlorosilane is 100-1000 μ L.
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Citations (5)
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| WO2007048921A1 (en) * | 2005-10-28 | 2007-05-03 | Agro Industrie Recherches Et Developpements A.R.D. | Use of a biomaterial for cleaning up contaminated environments |
| CN104945656A (en) * | 2015-06-25 | 2015-09-30 | 华南理工大学 | High-performance cellulose base oil absorption material and preparing method thereof |
| CN108479723A (en) * | 2018-05-04 | 2018-09-04 | 青岛塔山生态技术有限公司 | A kind of biomass environment-friendly oil absorption material and its preparation method and application |
| CN111330554A (en) * | 2020-03-24 | 2020-06-26 | 李娟� | Corn straw oil stain adsorbent for oil field and preparation method thereof |
| CN112156756A (en) * | 2020-10-12 | 2021-01-01 | 浙江农林大学 | Corn straw carbon-based nano adsorbent and preparation method thereof |
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- 2021-12-16 CN CN202111544932.9A patent/CN114225914B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007048921A1 (en) * | 2005-10-28 | 2007-05-03 | Agro Industrie Recherches Et Developpements A.R.D. | Use of a biomaterial for cleaning up contaminated environments |
| CN104945656A (en) * | 2015-06-25 | 2015-09-30 | 华南理工大学 | High-performance cellulose base oil absorption material and preparing method thereof |
| CN108479723A (en) * | 2018-05-04 | 2018-09-04 | 青岛塔山生态技术有限公司 | A kind of biomass environment-friendly oil absorption material and its preparation method and application |
| CN111330554A (en) * | 2020-03-24 | 2020-06-26 | 李娟� | Corn straw oil stain adsorbent for oil field and preparation method thereof |
| CN112156756A (en) * | 2020-10-12 | 2021-01-01 | 浙江农林大学 | Corn straw carbon-based nano adsorbent and preparation method thereof |
Non-Patent Citations (1)
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| 石彦龙等: "玉米秸秆油污吸附剂的制备及其在油水分离中的应用", 《科学通报》 * |
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