CN112473631A - Application of oil absorption material in wastewater treatment - Google Patents
Application of oil absorption material in wastewater treatment Download PDFInfo
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- CN112473631A CN112473631A CN202011313211.2A CN202011313211A CN112473631A CN 112473631 A CN112473631 A CN 112473631A CN 202011313211 A CN202011313211 A CN 202011313211A CN 112473631 A CN112473631 A CN 112473631A
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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
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/0202—Separation of non-miscible liquids by ab- or adsorption
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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
- B01J20/28002—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 physical properties
- B01J20/28011—Other properties, e.g. density, crush strength
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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
- B01J20/28047—Gels
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
-
- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
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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
- C02F2101/32—Hydrocarbons, e.g. oil
Abstract
The invention provides an application of an oil absorption material in wastewater treatment, wherein the oil absorption material is prepared from agricultural and forestry wastes as raw materials, is green and environment-friendly, and has good hydrophobic oil absorption performance. The invention carries out hydrophobic modification on agricultural and forestry wastes, thereby greatly improving the oil absorption effect. The oil absorption material is gel-like, has low density, can float on water surface, and is convenient to use and recover. The agricultural and forestry wastes are processed into coarse powder with the particle size of 1-10 mm and fine powder with the particle size of less than or equal to 100nm, so that the gel strength is increased, the service life is effectively prolonged, and the oil absorption effect is ensured. According to the invention, citric acid, inulin and the like are utilized to construct a gel system, so that a large number of hydrogen bonds have the effects of enhancing the gel strength, prolonging the service life of the oil absorption material and enhancing the oil absorption effect. The obtained material is also subjected to hydrophobic modification after demoulding, so that the hydrophobic effect is further improved, and the oil absorption effect is further improved.
Description
The application is a divisional application, the application number of the original application is 202010247295.8, the application date is 3/31/2020, and the name of the invention is 'an oil absorption material for wastewater treatment and a preparation method thereof'.
Technical Field
The invention relates to the technical field of wastewater treatment, in particular to application of an oil absorption material in wastewater treatment.
Background
In recent years, with the rapid development of modern industries and the continuous improvement of living standards of people, the production, transportation and use of petroleum and various oils have become a part of modern life. However, the problems of leakage accidents of oil tankers, discharge of industrial oily wastewater and the like are getting more and more serious. During the process of petroleum exploitation, transportation, loading and unloading, processing and use, oil tanker oil spill accidents and ship oily sewage discharge frequently occur, so that a great amount of marine organisms die, and unprecedented disasters are brought to economy and environment. In addition, an increasing number of industrial and municipal sewage and water-insoluble organic agents (including toluene, low molecular weight alkanes, halogenated hydrocarbons) are being improperly discharged, posing a threat to land and marine ecology. The removal of spilled oil and water-insoluble organic agents from the surface of water or other areas is a challenging task.
The currently common oil spill remediation methods include: in situ combustion, chemical methods (curing agents and dispersants), bioremediation methods, skimming, and absorption methods. However, in situ incineration and chemical dispersants can cause additional damage to the atmosphere and marine ecosystem because of the release of toxic gases and the synergistic toxicity of the oil and dispersant in the process. Bioremediation and skimming have limited oil absorption capacity and time consuming remediation processes. The oil-absorbing material can conveniently collect the spilled oil and thoroughly remove the oil or organic liquid pollutants on the water surface without generating adverse effect on ecology.
People continuously use porous substances such as plant straws, clay, sponge and the like as oil absorption materials, but the porous substances generally have the defects of low oil absorption, oil absorption and water absorption. Later, people synthesize a hydrophobic material by taking polypropylene as a main material, prepare an oil absorption pad with a certain shape and oil absorption viscosity, improve the oil-water selectivity to a certain extent, but have low oil absorption and poor oil retention performance, and can absorb a part of water when the oil-water is selectively absorbed. Then, people develop methacrylate oil absorption materials, and form three-dimensional reticular macromolecules through crosslinking, however, although the resin has good oil-water selectivity, the oil absorption multiplying power of the resin still cannot meet the ideal requirement, the oil absorption time is usually long, the saturated oil absorption can be achieved generally within several hours or even tens of hours, more importantly, the resin has a single oil absorption variety, only can absorb small-molecule oils, can hardly absorb large-molecule oils such as gasoline, diesel oil or vegetable oil commonly found in industrial wastewater, and can not absorb crude oil leaked on the ocean. From the perspective of environmental protection, natural biomass is used as a raw material, but plant cellulose has more hydroxyl groups and stronger hydrophilicity, so that the oil absorption capacity is weaker, the oil retention rate is poorer, and meanwhile, the floating performance is not good, so that the plant fiber needs to be modified to improve the oil absorption performance.
Patent CN106076266B discloses an oil absorption material, a preparation method and use thereof, which is prepared by mixing wood or agricultural waste with an acetylated modified lignin solution, but the oil absorption capacity of the oil absorption material obtained after the modification treatment is still very low, at most 18g/g, which is far from meeting the actual requirement of wastewater treatment.
Disclosure of Invention
The invention aims to provide the application of the oil absorption material in wastewater treatment, which takes agricultural and forestry wastes as raw materials, is green and environment-friendly, and has good hydrophobic oil absorption performance.
In order to achieve the purpose, the invention is realized by the following scheme:
a preparation method of an oil absorption material for wastewater treatment comprises the following specific steps in parts by weight:
(1) firstly, processing agricultural and forestry wastes into 1 part of coarse powder with the particle size of 1-10 mm and 1.5-2 parts of fine powder with the particle size of less than or equal to 100nm respectively, and then performing hydrophobic modification respectively to obtain hydrophobic coarse powder and hydrophobic fine powder for later use;
(2) then adding 4-5 parts of citric acid, 2-3 parts of inulin, hydrophobic fine powder and 0.8-1.5 parts of ferric nitrate into 20-30 parts of water, stirring and dissolving to obtain a premixed solution, and dropwise adding 25-28% of concentrated ammonia water to adjust the pH to be 7-8, so as to obtain a mixed solution;
(3) heating the mixed solution in a water bath at 85-95 ℃, violently stirring during heating, adding the hydrophobic coarse powder obtained in the step (1) when the mixed solution becomes sticky, continuously stirring until colloidal substances are generated, and continuously stirring until the colloidal substances are not increased any more to obtain mixed sol;
(4) and (3) molding by a mold, aging, carrying out vacuum freeze drying, demolding and carrying out hydrophobic modification to obtain the oil absorption material for wastewater treatment.
Preferably, in the step (1), the agricultural and forestry waste is selected from any one of straw stalks, corn stalks, sugar cane stalks or coconut shells.
Preferably, in the step (1), the agricultural and forestry waste is pretreated before being processed into coarse powder or fine powder, and the specific method is as follows: pouring agricultural and forestry wastes into a sodium hydroxide solution with the mass concentration of 10-15% and the weight of 5-8 times of that of the wastes, stirring for 15-18 hours, washing with water to be neutral, and drying to be constant in weight.
Preferably, in the step (1), the agricultural and forestry waste is directly processed into coarse powder by using a saw dust pulverizer.
Preferably, in the step (1), the preparation method of the fine powder is as follows: the agricultural and forestry wastes are firstly processed into coarse powder by a saw powder pulverizer, and then the coarse powder is processed into fine powder by a jet mill.
Preferably, in the step (1), the specific method for hydrophobic modification is as follows: adding the coarse powder or the fine powder into 3-aminopropyltriethoxysilane which is 3-5 times of the weight of the coarse powder or the fine powder, and mixing and stirring for 5-8 hours at the temperature of 130-140 ℃ and under the pressure of 0.2-0.3 MPa.
Preferably, the stirring speed in the step (3) is 5000-6000 r/min.
Preferably, in the step (4), the specific method for molding the mold is as follows: and pouring the mixed solvent into a mold for molding while the mixed solvent is hot, wherein the molding thickness is 3-5 mm.
Preferably, in the step (4), the aging process conditions are as follows: standing and aging for 8-10 hours at 20-30 ℃.
Preferably, in the step (4), the vacuum freeze-drying process conditions are as follows: freezing at the temperature of minus 40 ℃ to minus 50 ℃ for 10-12 hours, vacuumizing to 10-20 Pa, keeping the vacuum degree, heating to 20-30 ℃, and drying for 6-8 hours.
Preferably, in the step (4), the specific method for hydrophobic modification is as follows: and (3) soaking the demolded material in 5-8 times of 3-aminopropyltriethoxysilane by weight, treating the demolded material with 700-800W of microwave for 5-10 minutes, taking out the demolded material, and naturally drying the demolded material.
The oil absorption material for wastewater treatment is obtained by the preparation method.
The invention has the beneficial effects that:
the oil absorption material for wastewater treatment is prepared by taking agricultural and forestry wastes as raw materials, is green and environment-friendly, and has good hydrophobic oil absorption performance. The agricultural and forestry waste contains a large amount of cellulose components which are mainly in a thin-wall hollow form, has a porous structure and has a better adsorption effect theoretically, but has the defect of better hydrophilicity. The oil absorption material is gel-like, has low density, can float on water surface, and is convenient to use and recover.
The agricultural and forestry waste is processed into coarse powder with the particle size of 1-10 mm and fine powder with the particle size of less than or equal to 100nm, the oil absorption material is in a gel state, the addition of the coarse powder is favorable for increasing the gel strength so as to avoid damage in the using process, the service life is effectively prolonged, the consumption of the fine powder is slightly more, the distribution uniformity in a gel system is adjusted, and the oil absorption effect is ensured.
According to the invention, citric acid, inulin and the like are utilized to construct a gel system, and as citric acid and inulin contain a large amount of carboxylic acid or hydroxyl and the like, in the gelation process, a large amount of hydrogen bonds act to enhance the gel strength and prolong the service life of the oil absorption material, and more pores are formed inside along with the formation of the hydrogen bonds, so that the oil absorption effect is enhanced.
The obtained material is also subjected to hydrophobic modification after demoulding, so that the hydrophobic effect is further improved, and the oil absorption effect is further improved. According to the invention, the hydrophobic modification in the step (1) and the step (4) is realized by adopting 3-aminopropyltriethoxysilane, amino is introduced, and the amino can form hydrogen bonds with hydroxyl, carboxyl and the like in a system, so that the gel strength is further enhanced, the service life of the oil absorption material is prolonged, and the oil absorption effect is enhanced.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of an oil absorption material for wastewater treatment comprises the following specific steps:
(1) firstly, respectively processing agricultural and forestry wastes into 1kg coarse powder with the particle size of 1mm and 2kg fine powder with the particle size of 100nm, and then respectively carrying out hydrophobic modification to obtain hydrophobic coarse powder and hydrophobic fine powder for later use;
(2) then adding 4kg of citric acid, 3kg of inulin, the hydrophobic fine powder and 0.8kg of ferric nitrate into 30kg of water, stirring and dissolving to obtain a premixed solution, and dropwise adding 25% concentrated ammonia water with mass concentration to adjust the pH to be =8 to obtain a mixed solution;
(3) heating the mixed solution in a water bath at 85 ℃, violently stirring during heating, adding the hydrophobic coarse powder obtained in the step (1) after the mixed solution becomes viscous, continuously stirring until colloidal substances appear, and continuously stirring until the colloidal substances are not increased any more to obtain mixed sol;
(4) and (3) molding by a mold, aging, carrying out vacuum freeze drying, demolding and carrying out hydrophobic modification to obtain the oil absorption material for wastewater treatment.
In the step (1), the agricultural and forestry waste is corn stalks.
In the step (1), the agricultural and forestry waste is pretreated before being processed into coarse powder or fine powder, and the specific method comprises the following steps: pouring the agricultural and forestry waste into a sodium hydroxide solution with the mass concentration of 10% and the weight of 8 times of the agricultural and forestry waste, stirring for 18 hours, washing to be neutral, and drying to be constant in weight.
In the step (1), the agricultural and forestry wastes are directly processed into coarse powder by using a saw dust pulverizer.
In the step (1), the preparation method of the fine powder comprises the following steps: the agricultural and forestry wastes are firstly processed into coarse powder by a saw powder pulverizer, and then the coarse powder is processed into fine powder by a jet mill.
In the step (1), the specific method for hydrophobic modification is as follows: adding the coarse powder or the fine powder into 3 times of vinyl trimethoxy silane, and mixing and stirring for 8 hours at 140 ℃ and 0.2 MPa.
The stirring speed in the step (3) is 5000 r/min.
In the step (4), the specific method for molding the mold is as follows: pouring the mixed solvent into a mould for forming while the mixed solvent is hot, wherein the forming thickness is 5 mm.
In the step (4), the aging process conditions are as follows: standing and aging for 10 hours at 20 ℃.
In the step (4), the process conditions of vacuum freeze drying are as follows: freezing at-40 deg.C for 12 hr, vacuumizing to 10Pa, maintaining vacuum degree, heating to 30 deg.C, and drying for 6 hr.
In the step (4), the specific method for hydrophobic modification is as follows: and (3) soaking the demolded material in 8 times of weight of vinyl trimethoxy silane, treating for 10 minutes by 700W microwave, taking out and naturally drying.
Example 2
A preparation method of an oil absorption material for wastewater treatment comprises the following specific steps:
(1) firstly, processing agricultural and forestry wastes into 1kg coarse powder with the particle size of 10mm and 1.5kg fine powder with the particle size of 90nm respectively, and then performing hydrophobic modification respectively to obtain hydrophobic coarse powder and hydrophobic fine powder for later use;
(2) then adding 5kg of citric acid, 2kg of inulin, hydrophobic fine powder and 1.5kg of ferric nitrate into 20kg of water, stirring and dissolving to obtain a premixed solution, and dropwise adding concentrated ammonia water with the mass concentration of 28% to adjust the pH to be =7 to obtain a mixed solution;
(3) heating the mixed solution in a water bath at 95 ℃, violently stirring during heating, adding the hydrophobic coarse powder obtained in the step (1) after the mixed solution becomes viscous, continuously stirring until colloidal substances appear, and continuously stirring until the colloidal substances are not increased any more to obtain mixed sol;
(4) and (3) molding by a mold, aging, carrying out vacuum freeze drying, demolding and carrying out hydrophobic modification to obtain the oil absorption material for wastewater treatment.
In the step (1), the agricultural and forestry waste is sugarcane stalks.
In the step (1), the agricultural and forestry waste is pretreated before being processed into coarse powder or fine powder, and the specific method comprises the following steps: pouring the agricultural and forestry waste into a sodium hydroxide solution with the mass concentration of 15% and the weight of 5 times of the agricultural and forestry waste, stirring for 15 hours, washing to be neutral, and drying to be constant in weight.
In the step (1), the agricultural and forestry wastes are directly processed into coarse powder by using a saw dust pulverizer.
In the step (1), the preparation method of the fine powder comprises the following steps: the agricultural and forestry wastes are firstly processed into coarse powder by a saw powder pulverizer, and then the coarse powder is processed into fine powder by a jet mill.
In the step (1), the specific method for hydrophobic modification is as follows: adding the coarse powder or the fine powder into 5 times of 3-aminopropyltriethoxysilane by weight, and mixing and stirring at 130 deg.C and 0.3MPa for 5 hr.
The stirring speed in the step (3) is 6000 r/min.
In the step (4), the specific method for molding the mold is as follows: pouring the mixed solvent into a mould for forming while the mixed solvent is hot, wherein the forming thickness is 3 mm.
In the step (4), the aging process conditions are as follows: standing and aging for 8 hours at 30 ℃.
In the step (4), the process conditions of vacuum freeze drying are as follows: freezing at-50 deg.C for 10 hr, vacuumizing to 20Pa, maintaining vacuum degree, heating to 20 deg.C, and drying for 8 hr.
In the step (4), the specific method for hydrophobic modification is as follows: and (3) soaking the demolded material in 5 times of 3-aminopropyltriethoxysilane by weight, treating the demolded material for 5 minutes by 800W microwave, taking out the demolded material, and naturally drying the demolded material.
Example 3
A preparation method of an oil absorption material for wastewater treatment comprises the following specific steps:
(1) firstly, respectively processing agricultural and forestry wastes into 1kg coarse powder with the particle size of 5mm and 1.8kg fine powder with the particle size of 50nm, and then respectively carrying out hydrophobic modification to obtain hydrophobic coarse powder and hydrophobic fine powder for later use;
(2) then adding 4.5kg of citric acid, 2.5kg of inulin, hydrophobic fine powder and 1kg of ferric nitrate into 25kg of water, stirring and dissolving to obtain a premixed solution, and dropwise adding concentrated ammonia water with the mass concentration of 26% to adjust the pH to be =7.5 to obtain a mixed solution;
(3) heating the mixed solution in a water bath at 90 ℃, violently stirring during heating, adding the hydrophobic coarse powder obtained in the step (1) after the mixed solution becomes viscous, continuously stirring until colloidal substances appear, and continuously stirring until the colloidal substances are not increased any more to obtain mixed sol;
(4) and (3) molding by a mold, aging, carrying out vacuum freeze drying, demolding and carrying out hydrophobic modification to obtain the oil absorption material for wastewater treatment.
In the step (1), the agricultural and forestry waste is coconut shells.
In the step (1), the agricultural and forestry waste is pretreated before being processed into coarse powder or fine powder, and the specific method comprises the following steps: pouring the agricultural and forestry waste into 7 times of sodium hydroxide solution with the mass concentration of 12%, stirring for 16 hours, washing with water to be neutral, and drying to be constant in weight.
In the step (1), the agricultural and forestry wastes are directly processed into coarse powder by using a saw dust pulverizer.
In the step (1), the preparation method of the fine powder comprises the following steps: the agricultural and forestry wastes are firstly processed into coarse powder by a saw powder pulverizer, and then the coarse powder is processed into fine powder by a jet mill.
In the step (1), the specific method for hydrophobic modification is as follows: adding the coarse powder or the fine powder into 4 times of 3-aminopropyltriethoxysilane by weight, and mixing and stirring at 135 deg.C and 0.2MPa for 6 hr.
The stirring speed in the step (3) is 6000 r/min.
In the step (4), the specific method for molding the mold is as follows: pouring the mixed solvent into a mould for forming while the mixed solvent is hot, wherein the forming thickness is 4 mm.
In the step (4), the aging process conditions are as follows: standing and aging for 9 hours at 25 ℃.
In the step (4), the process conditions of vacuum freeze drying are as follows: freezing at-45 deg.C for 11 hr, vacuumizing to 15Pa, maintaining vacuum degree, heating to 25 deg.C, and drying for 7 hr.
In the step (4), the specific method for hydrophobic modification is as follows: and (3) soaking the demolded material in 6 times of 3-aminopropyltriethoxysilane by weight, treating for 8 minutes by 750W microwave, taking out and naturally drying.
Comparative example 1
A preparation method of an oil absorption material for wastewater treatment comprises the following specific steps:
(1) processing agricultural and forestry wastes into 2.8kg coarse powder with the particle size of 5mm, and then performing hydrophobic modification to obtain hydrophobic coarse powder for later use;
(2) then adding 4.5kg of citric acid, 2.5kg of inulin and 1kg of ferric nitrate into 25kg of water, stirring and dissolving to obtain a premixed solution, and dropwise adding concentrated ammonia water with the mass concentration of 26% to adjust the pH value to be =7.5 to obtain a mixed solution;
(3) heating the mixed solution in a water bath at 90 ℃, violently stirring during heating, adding the hydrophobic coarse powder obtained in the step (1) after the mixed solution becomes viscous, continuously stirring until colloidal substances appear, and continuously stirring until the colloidal substances are not increased any more to obtain mixed sol;
(4) and (3) molding by a mold, aging, carrying out vacuum freeze drying, demolding and carrying out hydrophobic modification to obtain the oil absorption material for wastewater treatment.
In the step (1), the agricultural and forestry waste is coconut shells.
In the step (1), the agricultural and forestry waste is pretreated before being processed into coarse powder, and the specific method comprises the following steps: pouring the agricultural and forestry waste into 7 times of sodium hydroxide solution with the mass concentration of 12%, stirring for 16 hours, washing with water to be neutral, and drying to be constant in weight.
In the step (1), the agricultural and forestry wastes are directly processed into coarse powder by using a saw dust pulverizer.
In the step (1), the specific method for hydrophobic modification is as follows: adding the coarse powder into 4 times of 3-aminopropyltriethoxysilane by weight, mixing and stirring at 135 deg.C and 0.2MPa for 6 hr.
The stirring speed in the step (3) is 6000 r/min.
In the step (4), the specific method for molding the mold is as follows: pouring the mixed solvent into a mould for forming while the mixed solvent is hot, wherein the forming thickness is 4 mm.
In the step (4), the aging process conditions are as follows: standing and aging for 9 hours at 25 ℃.
In the step (4), the process conditions of vacuum freeze drying are as follows: freezing at-45 deg.C for 11 hr, vacuumizing to 15Pa, maintaining vacuum degree, heating to 25 deg.C, and drying for 7 hr.
In the step (4), the specific method for hydrophobic modification is as follows: and (3) soaking the demolded material in 6 times of 3-aminopropyltriethoxysilane by weight, treating for 8 minutes by 750W microwave, taking out and naturally drying.
Comparative example 2
A preparation method of an oil absorption material for wastewater treatment comprises the following specific steps:
(1) firstly, processing agricultural and forestry wastes into 2.8kg of fine powder with the particle size of 50nm respectively, and then performing hydrophobic modification respectively to obtain hydrophobic fine powder for later use;
(2) then adding 4.5kg of citric acid, 2.5kg of inulin, hydrophobic fine powder and 1kg of ferric nitrate into 25kg of water, stirring and dissolving to obtain a premixed solution, and dropwise adding concentrated ammonia water with the mass concentration of 26% to adjust the pH to be =7.5 to obtain a mixed solution;
(3) heating the mixed solution in a water bath at 90 ℃, violently stirring during heating to generate colloid substances, and continuously stirring until the colloid substances are not increased any more to obtain mixed sol;
(4) and (3) molding by a mold, aging, carrying out vacuum freeze drying, demolding and carrying out hydrophobic modification to obtain the oil absorption material for wastewater treatment.
In the step (1), the agricultural and forestry waste is coconut shells.
In the step (1), the agricultural and forestry waste is pretreated before being processed into fine powder, and the specific method comprises the following steps: pouring the agricultural and forestry waste into 7 times of sodium hydroxide solution with the mass concentration of 12%, stirring for 16 hours, washing with water to be neutral, and drying to be constant in weight.
In the step (1), the preparation method of the fine powder comprises the following steps: the agricultural and forestry wastes are firstly processed into coarse powder by a saw powder pulverizer, and then the coarse powder is processed into fine powder by a jet mill.
In the step (1), the specific method for hydrophobic modification is as follows: adding the fine powder into 4 times of 3-aminopropyltriethoxysilane by weight, and mixing and stirring at 135 deg.C and 0.2MPa for 6 hr.
The stirring speed in the step (3) is 6000 r/min.
In the step (4), the specific method for molding the mold is as follows: pouring the mixed solvent into a mould for forming while the mixed solvent is hot, wherein the forming thickness is 4 mm.
In the step (4), the aging process conditions are as follows: standing and aging for 9 hours at 25 ℃.
In the step (4), the process conditions of vacuum freeze drying are as follows: freezing at-45 deg.C for 11 hr, vacuumizing to 15Pa, maintaining vacuum degree, heating to 25 deg.C, and drying for 7 hr.
In the step (4), the specific method for hydrophobic modification is as follows: and (3) soaking the demolded material in 6 times of 3-aminopropyltriethoxysilane by weight, treating for 8 minutes by 750W microwave, taking out and naturally drying.
Comparative example 3
A preparation method of an oil absorption material for wastewater treatment comprises the following specific steps:
(1) firstly, respectively processing agricultural and forestry wastes into 1kg coarse powder with the particle size of 5mm and 1.8kg fine powder with the particle size of 50nm, and then respectively carrying out hydrophobic modification to obtain hydrophobic coarse powder and hydrophobic fine powder for later use;
(2) then adding 7kg of citric acid, the hydrophobic fine powder and 1kg of ferric nitrate into 25kg of water, stirring and dissolving to obtain a premixed solution, and dropwise adding concentrated ammonia water with the mass concentration of 26% to adjust the pH to be =7.5 to obtain a mixed solution;
(3) heating the mixed solution in a water bath at 90 ℃, violently stirring during heating, adding the hydrophobic coarse powder obtained in the step (1) after the mixed solution becomes viscous, continuously stirring until colloidal substances appear, and continuously stirring until the colloidal substances are not increased any more to obtain mixed sol;
(4) and (3) molding by a mold, aging, carrying out vacuum freeze drying, demolding and carrying out hydrophobic modification to obtain the oil absorption material for wastewater treatment.
In the step (1), the agricultural and forestry waste is coconut shells.
In the step (1), the agricultural and forestry waste is pretreated before being processed into coarse powder or fine powder, and the specific method comprises the following steps: pouring the agricultural and forestry waste into 7 times of sodium hydroxide solution with the mass concentration of 12%, stirring for 16 hours, washing with water to be neutral, and drying to be constant in weight.
In the step (1), the agricultural and forestry wastes are directly processed into coarse powder by using a saw dust pulverizer.
In the step (1), the preparation method of the fine powder comprises the following steps: the agricultural and forestry wastes are firstly processed into coarse powder by a saw powder pulverizer, and then the coarse powder is processed into fine powder by a jet mill.
In the step (1), the specific method for hydrophobic modification is as follows: adding the coarse powder or the fine powder into 4 times of 3-aminopropyltriethoxysilane by weight, and mixing and stirring at 135 deg.C and 0.2MPa for 6 hr.
The stirring speed in the step (3) is 6000 r/min.
In the step (4), the specific method for molding the mold is as follows: pouring the mixed solvent into a mould for forming while the mixed solvent is hot, wherein the forming thickness is 4 mm.
In the step (4), the aging process conditions are as follows: standing and aging for 9 hours at 25 ℃.
In the step (4), the process conditions of vacuum freeze drying are as follows: freezing at-45 deg.C for 11 hr, vacuumizing to 15Pa, maintaining vacuum degree, heating to 25 deg.C, and drying for 7 hr.
In the step (4), the specific method for hydrophobic modification is as follows: and (3) soaking the demolded material in 6 times of 3-aminopropyltriethoxysilane by weight, treating for 8 minutes by 750W microwave, taking out and naturally drying.
Test examples
1. Examination of gel Strength
The gel strength of the oil-absorbing materials obtained in examples 1 to 3 and comparative examples 2 and 3 was examined, and the results are shown in Table 1.
The impact strength is detected by adopting an impact strength tester (KCJ-50 type cang, Koxing instruments and equipment Co., Ltd.), the bending strength is detected by adopting an HY-0580 electronic universal material tester (Shanghai Hengyi precision instruments Co., Ltd.), and relevant detection is carried out according to the instrument instruction.
TABLE 1 gel Strength examination results
| Impact strength (KJ/m)2） | Flexural strength (MPa) | |
| Example 1 | 685 | 603 |
| Example 2 | 753 | 712 |
| Example 3 | 762 | 720 |
| Comparative example 2 | 586 | 493 |
| Comparative example 3 | 595 | 510 |
As can be seen from Table 1, the oil-absorbing materials obtained in examples 1-3 have ideal gel strength, wherein in example 1, vinyltrimethoxysilane is used for hydrophobic modification, so that the formation of hydrogen bonds is reduced, and the gel strength is slightly poor. Comparative example 2, in which the coarse powder was replaced with the fine powder, had poor gel strength, and comparative example 3, in which the inulin was replaced with citric acid, had poor gelation degree and also poor gel strength.
2. Investigation of hydrophobic oil absorption Properties
The hydrophobic oil absorption performance of the oil absorption materials obtained in examples 1-3 and comparative examples 1 and 3 is examined, and the results are shown in Table 2.
The contact angle was measured using an OCA15Pro type video optical contact angle measuring instrument. The measurement conditions were: the injection needle model was SNS 052/026, the volume of the injection droplet (water) was 1 μ L, and the liquid profile fitting calculation used the ellipsometry. And (4) performing measurement after tabletting, selecting three different positions on the sample for measurement, and recording the intermediate value as the final experimental result.
TABLE 2 investigation of hydrophobic oil absorption Properties
| Contact angle (°) | Oil absorption multiplying power (toluene, g/g) | Oil absorption multiplying power (diesel oil, g/g) | |
| Example 1 | 149.3 | 45.8 | 48.3 |
| Example 2 | 156.8 | 67.2 | 68.8 |
| Example 3 | 158.2 | 68.3 | 69.1 |
| Comparative example 1 | 148.3 | 41.5 | 40.3 |
| Comparative example 3 | 149.1 | 35.8 | 36.2 |
As can be seen from Table 2, the oil absorption materials obtained in the examples 1-3 have large contact angles, good hydrophobicity, higher oil absorption multiplying power for toluene and diesel oil and good oil absorption effect, wherein the example 1 utilizes vinyl trimethoxy silane for hydrophobic modification, the contact angles are slightly small, hydrogen bond formation is reduced, and the oil absorption multiplying power is obviously low. Comparative example 1, replacing the fine powder with coarse powder, had poor oil absorption effect, and comparative example 3, replacing inulin with citric acid, had poor gelation degree and poor oil absorption effect.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (6)
1. The application of the oil absorption material in wastewater treatment is characterized in that the preparation method of the oil absorption material comprises the following specific steps in parts by weight:
(1) firstly, processing agricultural and forestry wastes into 1 part of coarse powder with the particle size of 1-10 mm and 1.5-2 parts of fine powder with the particle size of less than or equal to 100nm respectively, and then performing hydrophobic modification respectively to obtain hydrophobic coarse powder and hydrophobic fine powder for later use; the specific method for hydrophobic modification is as follows: adding the coarse powder or the fine powder into 3-aminopropyltriethoxysilane which is 3-5 times of the weight of the coarse powder or the fine powder, and mixing and stirring for 5-8 hours at the temperature of 130-140 ℃ and under the pressure of 0.2-0.3 MPa; the agricultural and forestry waste is selected from any one of straw stalks, corn stalks, bagasse or coconut coir;
(2) then adding 4-5 parts of citric acid, 2-3 parts of inulin, hydrophobic fine powder and 0.8-1.5 parts of ferric nitrate into 20-30 parts of water, stirring and dissolving to obtain a premixed solution, and dropwise adding 25-28% of concentrated ammonia water to adjust the pH to be 7-8, so as to obtain a mixed solution;
(3) heating the mixed solution in a water bath at 85-95 ℃, violently stirring during heating, adding the hydrophobic coarse powder obtained in the step (1) when the mixed solution becomes sticky, continuously stirring until colloidal substances are generated, and continuously stirring until the colloidal substances are not increased any more to obtain mixed sol;
(4) molding a mould, aging, carrying out vacuum freeze drying, demoulding and hydrophobic modification to obtain the oil absorption material for wastewater treatment; the specific method for hydrophobic modification is as follows: and (3) soaking the demolded material in 5-8 times of 3-aminopropyltriethoxysilane by weight, treating the demolded material with 700-800W of microwave for 5-10 minutes, taking out the demolded material, and naturally drying the demolded material.
2. The use of claim 1, wherein in the step (1), the agricultural and forestry waste is pretreated before being processed into coarse powder or fine powder by the following specific method: pouring agricultural and forestry wastes into a sodium hydroxide solution with the mass concentration of 10-15% and the weight of 5-8 times of that of the wastes, stirring for 15-18 hours, washing with water to be neutral, and drying to be constant in weight.
3. The use of claim 1, wherein in step (1), the agricultural and forestry waste is processed into coarse powder directly by using a saw-dust pulverizer.
4. The use according to claim 1, wherein in step (1), the fine powder is prepared by the following method: the agricultural and forestry wastes are firstly processed into coarse powder by a saw powder pulverizer, and then the coarse powder is processed into fine powder by a jet mill.
5. Use according to any one of claims 1 to 4, wherein in step (4) the aging process conditions are: standing and aging for 8-10 hours at 20-30 ℃.
6. The use according to any one of claims 1 to 5, wherein in step (4), the vacuum freeze-drying process conditions are as follows: freezing at the temperature of minus 40 ℃ to minus 50 ℃ for 10-12 hours, vacuumizing to 10-20 Pa, keeping the vacuum degree, heating to 20-30 ℃, and drying for 6-8 hours.
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