CN111056646A - Preparation method of floatable particles - Google Patents
Preparation method of floatable particles Download PDFInfo
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- CN111056646A CN111056646A CN201911000661.3A CN201911000661A CN111056646A CN 111056646 A CN111056646 A CN 111056646A CN 201911000661 A CN201911000661 A CN 201911000661A CN 111056646 A CN111056646 A CN 111056646A
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- Prior art keywords
- sodium alginate
- aqueous solution
- floatable
- preparation
- calcium chloride
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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
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/34—Biological treatment of water, waste water, or sewage characterised by the microorganisms used
- C02F3/343—Biological treatment of water, waste water, or sewage characterised by the microorganisms used for digestion of grease, fat, oil
-
- E—FIXED CONSTRUCTIONS
- E02—HYDRAULIC ENGINEERING; FOUNDATIONS; SOIL SHIFTING
- E02B—HYDRAULIC ENGINEERING
- E02B15/00—Cleaning or keeping clear the surface of open water; Apparatus therefor
- E02B15/04—Devices for cleaning or keeping clear the surface of open water from oil or like floating materials by separating or removing these materials
- E02B15/041—Devices for distributing materials, e.g. absorbed or magnetic particles over a surface of open water to remove the oil, with or without means for picking up the treated oil
-
- 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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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/08—Seawater, e.g. for desalination
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/20—Controlling water pollution; Waste water treatment
- Y02A20/204—Keeping clear the surface of open water from oil spills
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- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Engineering & Computer Science (AREA)
- Microbiology (AREA)
- Chemical & Material Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Hydrology & Water Resources (AREA)
- Biodiversity & Conservation Biology (AREA)
- Organic Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Mechanical Engineering (AREA)
- Civil Engineering (AREA)
- Structural Engineering (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Materials For Medical Uses (AREA)
- Medicinal Preparation (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention discloses a preparation method of floatable particles. The method comprises the steps of adding an aqueous solution containing sodium alginate, an auxiliary agent or ethyl cellulose into an aqueous solution of calcium chloride, and crosslinking and solidifying at a certain temperature to obtain particles capable of floating on the surface of a seawater or seawater oil layer. In the preparation method of the floatable particles, the concentration of the sodium alginate is 1-3wt%, the mass ratio of the auxiliary agent to the sodium alginate is 1:10-1:100, the mass ratio of the sodium alginate to the ethyl cellulose is 1:0.3-1:6, and the concentration of the calcium chloride aqueous solution is 0.10-0.35 mol.L‑1The reaction temperature is 25-80 ℃ and the reaction time is 3-10 minutes. The preparation method of the floatable particles provided by the invention is beneficial to bacteriaThe growth and concentration of the flora are improved, the flora and the oil drops are effectively contacted, and the preparation method has the characteristics of simple and quick preparation, low cost, easy amplification and field preparation, no secondary pollution and the like.
Description
Technical Field
The invention belongs to the technical fields of chemical industry, environmental protection and ocean, and particularly relates to a preparation method of floatable particles.
Background
Offshore oil spill caused by oil leakage and discharge caused by the exploitation, shipping, pipe transportation and offshore storage activities of offshore oil is the most serious problem of global marine pollution at present.
Current methods of treating marine oil spills include primarily physical, chemical, and biological methods. The physical method can mainly remove most of the oil spillage, but still remains a plurality of oil spillage pollutants which cannot be effectively treated; the chemical method generally adopts a chemical dispersant to emulsify and disperse crude oil, and can disperse oil spill into smaller droplets, but the oil spill is not completely removed; the oil spill pollutant is treated by biological method by putting pollutant-degrading bacteria into oil spill seawater, adding nutrient substances or biosurfactant into the seawater to promote the rapid growth of the pollutant-degrading bacteria, or degrading the oil spill by utilizing microbial metabolism. The biological method can degrade the oil spill pollutants through microorganisms, solves the problem that residual oil spill cannot be removed by physical and chemical methods, and is a green method for solving marine oil spill pollution and restoring ecological environment.
However, the openness and fluidity of the ocean results in dilution or loss of the nutrient substrates and strains directly delivered to the ocean. Meanwhile, the oil film floating on the water surface is also broken or converged and is continuously changed along with the movement of sea waves. The microbial flora and the nutrient concentration have influence on the natural degradation of the spilled oil, but are closely related to the contact effectiveness of the microbes and oil drops, the effective solution is to limit the high-concentration flora and the nutrient substrate in a certain space, the flora space is required to float and move along with an oil film, and the preparation of the floatable and biocompatible material or medium is a feasible method for solving the marine spilled oil.
The sodium alginate and cellulose have wide sources, the materials are easy to obtain, the biocompatibility is good, secondary pollution can not be caused, and the obtained particles which can float or suspend on the surface of the seawater or the seawater oil layer have the characteristics of simple and rapid preparation and the like, and have not been reported yet.
Disclosure of Invention
In view of the above problems in the prior art, the present invention aims to provide a method for preparing floatable particles.
The preparation method of the floatable particles is characterized in that an aqueous solution containing sodium alginate, an auxiliary agent or ethyl cellulose is added into a calcium chloride aqueous solution, and crosslinking and solidification are carried out at a certain temperature to obtain the floatable particles capable of floating or suspending on the surface of seawater or a seawater oil layer.
The preparation method of the floatable particle is characterized by comprising the following preparation steps of:
1) preparing a sodium alginate aqueous solution;
2) adding an auxiliary agent or ethyl cellulose into the sodium alginate aqueous solution obtained in the step 1);
3) dripping the sodium alginate aqueous solution obtained in the step 2) into the calcium chloride aqueous solution, and filtering or fishing out after crosslinking and curing at a certain temperature to obtain the floatable particles.
The preparation method of the floatable particles is characterized in that the concentration of the sodium alginate aqueous solution in the step 1) is 1-3 wt%.
The preparation method of the floatable particles is characterized in that the auxiliary agent in the step 2) is ammonium carbonate, ammonium bicarbonate, sodium bicarbonate, ammonium nitrite or ammonium carbamate, and the feeding mass ratio of the auxiliary agent to the sodium alginate is 1: 10-100.
The preparation method of the floatable particles is characterized in that the mass ratio of the sodium alginate to the ethyl cellulose in the step 2) is 1:0.3-1: 6.
The preparation method of the floatable particles is characterized in that the concentration of the calcium chloride aqueous solution in the step 3) is 0.10-0.35 mol.L-1The mass ratio of sodium alginate to calcium chloride is 1:1.5-1:40, and the mass of calcium chloride is the mass of solute.
The preparation method of the floatable particles is characterized in that the temperature of the crosslinking curing reaction in the step 3) is 25-80 ℃, and the reaction time is 3-10 minutes.
The floatable particles obtained by the preparation method have the particle size of 2.0-5.0 mm, and the floating or suspending time of the particles on the surface of seawater or the surface of a seawater oil layer is 1h-8 d.
By adopting the technology, compared with the prior art, the invention has the following beneficial effects: according to the preparation method of the floatable particles, provided by the invention, the sodium alginate, the auxiliary agent or the ethyl cellulose are used as the matrix, so that the biocompatibility is good, the material is easy to obtain, no secondary pollution is caused, the preparation is simple and quick, the cost is low, and the amplification and field preparation are easy; the prepared particles can float or suspend on the surface of seawater or a seawater oil layer, so that biological flora and a substrate can be limited in a certain space along with the movement of sea waves, the effective contact between the flora and oil drops is facilitated, and the growth of the flora and the improvement of the concentration can be effectively promoted.
Detailed Description
The invention will be further described with reference to specific examples, but the scope of the invention is not limited thereto:
example 1
Dissolving 1.0 g of sodium alginate in 99 ml of water, adding 0.1 g of ammonium carbonate into the sodium alginate aqueous solution, stirring for about 2 minutes to prepare a uniform solution, and then dripping the solution into a container containing 0.25 mol.L of sodium alginate at 80 DEG C-1And (3) carrying out constant temperature for 10 minutes in a calcium chloride solution, crosslinking and curing, and filtering to obtain a class of floating particles with uniform particle size, wherein the average particle size of the particles is 2.87mm, the maximum particle size is 3.14mm, the minimum particle size is 2.53mm, and the floating particles can float in seawater for 5 days.
Example 2
Dissolving 2.0 g of sodium alginate in 98 ml of water, adding 0.02 g of ammonium bicarbonate into the sodium alginate aqueous solution, stirring for about 2 minutes to prepare a uniform solution, and then flowing the solution through a microchannel reactor to be dropped into 0.25 mol.L of solution at 40 DEG C-1And (3) carrying out constant temperature for 8 minutes in the calcium chloride solution, crosslinking and curing, and filtering to obtain a class of floating particles with uniform particle size, wherein the average particle size of the particles is 3.61mm, the maximum particle size is 3.97mm, the minimum particle size is 3.34mm, and the floating particles can float in seawater for 3 days.
Example 3
Dissolving 3.0 g of sodium alginate in 97 ml of water, adding 0.04 g of ammonium carbonate into the sodium alginate aqueous solution, stirring for about 2 minutes to prepare a uniform solution, and then dropping the solution into 0.30 mol.L of solution at 70 ℃ through a microchannel reactor-1And (3) carrying out constant temperature for 5 minutes in the calcium chloride solution, crosslinking and curing, and filtering to obtain the floating particles with uniform particle size. The average particle diameter of the granules is 3.73mm, the maximum particle diameter is 4.01mm, and the minimum particle diameter3.45mm, and can float in seawater for 3 days.
Example 4
Dissolving 1.0 g of sodium alginate in 98 ml of water, selecting powdered ethyl cellulose with the relative viscosity of 90-110mpa.s as a raw material, continuously adding 1.0 g of ethyl cellulose into the sodium alginate aqueous solution under the stirring state, and stirring for about 5 minutes to uniformly mix the ethyl cellulose into the solution. Then 0.04 g of ammonium carbamate is added into the mixed solution, and the mixed solution is stirred for about 2 minutes to prepare a uniform solution. Then the solution is dropped into a 0.30 mol.L solution filled with a solution at 40 ℃ through a micro-tube reactor-1And (3) carrying out constant temperature for 5 minutes in the calcium chloride solution, crosslinking and curing, and filtering to obtain the floating particles with uniform particle size. The average particle size of the granules is 3.57mm, the maximum particle size is 3.90mm, the minimum particle size is 3.12mm, and the granules can float in seawater for 10 days.
Example 5
Dissolving 2.0 g of sodium alginate in 97 ml of water, selecting powdered ethyl cellulose with relative viscosity of 90-110mpa.s as a raw material, continuously adding 1.0 g of ethyl cellulose into the sodium alginate aqueous solution under stirring, and stirring for about 5 minutes to uniformly mix the ethyl cellulose into the solution. Then, 0.08 g of sodium bicarbonate was added to the mixed solution, and stirred for about 2 minutes to prepare a uniform solution. Then the solution is dropped into a 0.25 mol.L solution filled with a solution at 80 ℃ through a micro-tube reactor-1And (3) carrying out constant temperature for 3 minutes in the calcium chloride solution, crosslinking and curing, and filtering to obtain the floating particles with uniform particle size. The average particle size of the granules is 4.25mm, the maximum particle size is 3.29mm, the minimum particle size is 3.84mm, and the granules can float in seawater for 6 days.
Example 6
Dissolving 2.0 g of sodium alginate in 96 ml of water, selecting powdered ethyl cellulose with the relative viscosity of 90-110mpa.s as a raw material, continuously adding 2.0 g of ethyl cellulose into the sodium alginate aqueous solution under the stirring state, and stirring for about 5 minutes to uniformly mix the ethyl cellulose into the solution. Then 0.21 g of ammonium nitrite is added into the mixed solution, and the mixed solution is stirred for about 2 minutes to prepare a uniform solution. Then the solution is dropped into a container with 0.25 mol.L at 25 DEG C-1In calcium chloride solution, the calcium chloride solution is filtered out after being cross-linked and solidified for 6 minutes at constant temperature to obtain a first-class particleFloating particles with uniform diameter. The average particle size of the granules is 3.84mm, the maximum particle size is 4.27mm, the minimum particle size is 3.53mm, and the granules can float in seawater for 8 days.
Example 7
Dissolving 1.0 g of sodium alginate in 97 ml of water, selecting powdered ethyl cellulose with relative viscosity of 90-110mpa.s as a raw material, continuously adding 2.0 g of ethyl cellulose into the sodium alginate aqueous solution under stirring, and stirring for about 5 minutes to uniformly mix the ethyl cellulose into the solution. Then the solution flows through a micro-tube reactor and is dropped into a micro-tube reactor which is filled with 0.15 mol.L solution at 25 DEG C-1The calcium chloride solution is filtered out after crosslinking and curing for 10 minutes at room temperature, and a class of floating particles with uniform particle size are obtained. The average particle size of the granules is 3.63mm, the maximum particle size is 4.03mm, the minimum particle size is 3.17mm, and the granules can float in seawater for 6 days.
Example 8
Dissolving 2.0 g of sodium alginate in 97 ml of water, selecting powdered ethyl cellulose with relative viscosity of 90-110mpa.s as a raw material, continuously adding 1.0 g of ethyl cellulose into the sodium alginate aqueous solution under stirring, and stirring for about 5 minutes to uniformly mix the ethyl cellulose into the solution. Then the solution is dropped into 0.20 mol.L-1 calcium chloride solution with the temperature of 25 ℃, and is filtered out after 4 minutes of crosslinking and solidification under the state of room temperature, so as to obtain a class of floating particles with uniform particle size. The average particle size of the granules is 3.90mm, the maximum particle size is 4.28mm, the minimum particle size is 3.64mm, and the granules can float in seawater for 3 days.
Example 9
Dissolving 3.0 g of sodium alginate in 95 ml of water, selecting powdered ethyl cellulose with the relative viscosity of 90-110mpa.s as a raw material, continuously adding 2.0 g of ethyl cellulose into the sodium alginate aqueous solution under the stirring state, and stirring for about 5 minutes to uniformly mix the ethyl cellulose into the solution. Then the solution is dropped into a container with 0.30 mol.L at 20 DEG C-1The calcium chloride solution is filtered out after 3 minutes of crosslinking and curing at room temperature, and a class of floating particles with uniform particle size are obtained. The average particle size of the granules is 3.86mm, the maximum particle size is 4.10mm, the minimum particle size is 3.55mm, and the granules can float in seawater for 6 days.
Claims (8)
1. A process for preparing the floatable particles includes such steps as adding the aqueous solution containing sodium alginate, assistant or ethyl cellulose to the aqueous solution of calcium chloride, cross-linking at a certain temp for solidifying to obtain the floatable particles able to float or suspend on the surface of seawater or oil layer.
2. A method of preparing a floatable particle according to claim 1, characterized by comprising the steps of:
1) preparing a sodium alginate aqueous solution;
2) adding an auxiliary agent or ethyl cellulose into the sodium alginate aqueous solution obtained in the step 1);
3) dripping the sodium alginate aqueous solution obtained in the step 2) into the calcium chloride aqueous solution, and filtering or fishing out after crosslinking and curing at a certain temperature to obtain the floatable particles.
3. A process for the preparation of floatable granules according to claim 2, characterised in that the concentration of the aqueous solution of sodium alginate in step 1) is 1-3% by weight.
4. The method for preparing floatable particles according to claim 2, characterized in that the adjuvant in step 2) is ammonium carbonate, ammonium bicarbonate, sodium bicarbonate, ammonium nitrite or ammonium carbamate, and the feeding mass ratio of the adjuvant to sodium alginate is 1: 10-100.
5. The process for the preparation of floatable granules according to claim 2, characterized in that the mass ratio of sodium alginate to ethylcellulose in step 2) is 1:0.3-1: 6.
6. The process for producing a floatable granule according to claim 2, characterized in that the concentration of the aqueous solution of calcium chloride in the step 3) is 0.10 to 0.35 mol-L-1The mass ratio of the sodium alginate to the calcium chloride is 1:1.5-1: 40.
7. A method of producing floatable particles according to claim 2, characterized in that the temperature of the cross-linking curing reaction in step 3) is 25-80 ℃ and the reaction time is 3-10 minutes.
8. A floatable granule obtained by the production method according to any one of claims 1 to 7, having a particle size of 2.0 to 5.0 mm and having a floating or suspending time on the surface of seawater or a layer of seawater oil of 1h to 8 d.
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