CN110038324B - Magnetic fireproof oil-absorbing porous silicon rubber material and preparation method and application thereof - Google Patents
Magnetic fireproof oil-absorbing porous silicon rubber material and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of oil absorption materials, and particularly relates to a magnetic fireproof oil absorption porous silicon rubber material and a preparation method and application thereof. The hydrophobic porous silicone rubber material which has quick magnetic response, is fireproof and can be recycled is prepared by adopting a simple and green synthesis method, the adopted raw materials are low in price and easy to obtain, and the synthesis method is simple. The prepared material has good hydrophobic property and good fireproof effect, does not drop combustion molten drops, and has quick magnetic response property, so that large-scale production is easy to realize.
Description
Technical Field
The invention belongs to the technical field of oil absorption materials, and particularly relates to a magnetic, fireproof and recyclable porous silicon rubber material which is controllable in magnetism, can operate in a dangerous environment and is simple to synthesize.
Background
With the rapid development of industrialization, the leakage of petroleum and organic solvents frequently occurs, which not only brings huge economic loss, but also brings huge environmental pollution. The traditional leakage treatment method has low efficiency and consumes a great deal of manpower and financial resources. A large number of highly effective oil absorbing materials have emerged in recent years, such as: cellulose aerogel, graphene aerogel, inorganic nano-film and the like, but the complex preparation process is not suitable for large-scale preparation and use. Chinese patent publication No. CN106519284A discloses a novel porous silicone rubber for oil-water separation, which is prepared by curing silicone rubber and NaCl to prepare a porous hydrophobic silicone rubber material, which can realize continuous separation and recovery of oil phase and improve the separation efficiency of oil stain, but like most oil-absorbing materials, the adsorption and separation capacity may be reduced after long-term use, and the post-recovery treatment is troublesome and the cost is high. Meanwhile, as leaked petroleum and organic solvents are easy to combust and explode, the common oil absorption material does not have strong fire resistance, and a fire-resistant oil absorption material is needed to be found in some dangerous areas which are not suitable for personnel to work.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of a magnetic, fireproof and recyclable porous silicon rubber material.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a magnetic fireproof oil-absorption porous silicon rubber material comprises the following steps:
(1) dissolving soluble salt of zinc and soluble salt of iron into distilled water, adjusting pH to be alkaline by using sodium hydroxide with certain concentration, stirring and reacting for 1-3h in a water bath kettle at 60-80 ℃ to obtain a mixed solution, carrying out suction filtration on the mixed solution, washing for a plurality of times by using distilled water, drying to obtain a precursor, and finally calcining to obtain powdery Zinc Ferrite (ZFO) nano particles;
(2) and (2) uniformly dispersing sodium chloride and the zinc ferrite nano particles obtained in the step (1) into the prepolymer, adding a curing agent, uniformly mixing, curing, cooling to room temperature, soaking in hot water to remove the sodium chloride particles, and drying to obtain the magnetic fire-resistant oil-absorbing porous silicon rubber material.
Further, the soluble salt of zinc in the step (1) is Zn (NO)3)2·6H2O, soluble salts of iron being Fe (NO)3)3·9H2And O, wherein the molar ratio of the soluble salt of zinc to the soluble salt of iron is 1 (1-2).
Further, in the step (1), the drying time is 1-3h, the drying temperature is 50-70 ℃, the calcination time is 3-6h, and the calcination temperature is 380-420 ℃.
Further, the prepolymer in the step (2) is polydimethylsiloxane; the curing agent is Dow Corning SYLGARD 184.
Further, the mass ratio of the sodium chloride to the prepolymer in the step (2) is (5-9): 1.
further, in the step (2), the mass ratio of the zinc ferrite nano particles to the prepolymer is 1: (8-10).
Further, in the step (2), the mass ratio of the curing agent to the prepolymer is 1: (10-12).
Further, the curing time in the step (2) is 1-3h, and the curing temperature is 180-; the soaking temperature is 80-95 ℃, and the soaking time is 12-36 h; the drying temperature is 80-100 ℃.
The preparation process comprises the steps of preparing Zinc Ferrite (ZFO) nanoparticles by a two-step method, and mixing sodium chloride particles, zinc ferrite nanoparticles, prepolymer and curing agent to obtain the recyclable magnetic fire-resistant oil-absorbing porous silicon rubber material with hydrophobic property.
The application of the magnetic fireproof oil absorption porous silicon rubber material in preparing a fireproof oil absorption material.
The invention has the beneficial effects that:
1. the preparation method is easy to popularize on a large scale, the preparation process is green and environment-friendly, the raw materials are cheap and easy to obtain, and the preparation process is simple. The magnetic fireproof oil-absorption porous silicon rubber material prepared by the invention has good hydrophobic oil-absorption property.
2. The prepared material has quick magnetic response performance, so that the material is wider in application places, manual contact is not needed, and the prepared material can be placed in a remote and dangerous operation area only under the condition of an external magnetic field, so that the harm to personnel is reduced, and the waste of human resources is avoided.
3. From the viewpoint of fire resistance, we used commercially available polyurethane sponge as reference, and through the burning test, we found that the prepared rubber material has good fire resistance effect, the prepared material burns slowly (fig. 3b, c) and has a large amount of residue (fig. 3b, d), while the commercially available polyurethane sponge burns violently immediately after being ignited (fig. 3a, c) and burns out with almost no residue (fig. 3a, d), which indicates that the material prepared by the present invention has good fire resistance performance, and can reduce the hazard caused by fire during the rescue process of leakage accident.
4. The invention has good stability, and the material prepared by the invention still keeps good adsorption capacity after being soaked in ultraviolet, strong acid, strong base and salt solution (figure 4).
5. The material prepared by the invention can be recycled, and has no obvious influence on the oil adsorption performance after being recycled for many times, the oil product can be recovered only by simple extrusion, the operation is simple, and the cost is low.
Drawings
In fig. 1, a is a scanning electron microscope picture of the magnetic fire-resistant oil-absorbing porous silicone rubber material prepared in example 1; b is a photograph of the contact angle of the material prepared in example 1 with water; c is an optical photograph of the water droplets forming a nearly spherical shape on the surface of the material prepared in example 1;
in fig. 2, a is an optical photograph of the magnetic refractory oil-absorbing porous silicone rubber material prepared in example 1 adsorbed by a magnet, and b is a magnetic hysteresis chart of the material prepared in example 1;
FIG. 3A is an optical photograph showing the burning of a commercially available polyurethane sponge (PU); b is a combustion optical photograph of the magnetic fire-resistant oil-absorbing porous silicon rubber material prepared in example 1; c is the heat release rate of the commercial polyurethane sponge (PU) and the material prepared in example 1, d is the mass residual percentage of the commercial polyurethane sponge (PU) and the material prepared in example 1;
fig. 4 is an optical photograph of the magnetic fire-resistant oil-absorbing porous silicone rubber material prepared in example 1 after being soaked in 2M sodium hydroxide (left in fig. 3), 2M hydrochloric acid (in fig. 3) and a saturated sodium chloride solution (right in fig. 3), respectively, for 2 hours;
in fig. 5, a, b and c are optical photographs of the magnetic fireproof oil-absorbing porous silicone rubber material prepared in example 1 immersed in ethanol, acetone and dimethyl sulfoxide solvents respectively; e. f and g are circulation curves of soaking the material prepared in the embodiment 1 in ethanol, acetone and dimethyl sulfoxide solvents for 3 hours, drying and compressing for 100 times respectively;
in fig. 6, a is an optical photograph of a tensile test of the magnetic fire-resistant oil-absorbing porous silicone rubber material prepared in example 1, and b is a breaking elongation curve of the material prepared in example 1.
Detailed Description
The technical solution of the present invention will be further described in detail with reference to the following examples, wherein the curing agent used in the following examples is Dow Corning SYLGARD 184, and Polydimethylsiloxane (PDMS) is a common commercially available product.
Example 1
A preparation method of a magnetic fireproof oil-absorption porous silicon rubber material comprises the following steps:
(1) 20 mmol of Zn (NO)3)2·6H2O and 40 mmol of Fe (NO)3)3·9H2Dissolving O in distilled water, adjusting the pH value to 12 by using 5 mol/L sodium hydroxide, stirring for 1h in a water bath kettle at 60 ℃ to obtain a mixed solution, carrying out suction filtration on the mixed solution, washing for a plurality of times by using distilled water, drying for 3h in an oven at 60 ℃ to obtain a precursor, and finally calcining for 4h at 400 ℃ to obtain powdery Zinc Ferrite (ZFO) nanoparticles;
(2) adding 36g of sodium chloride particles and 0.4g of zinc ferrite nanoparticles into 4g of polydimethylsiloxane prepolymer, stirring and mixing uniformly, adding 0.4g of curing agent, then curing at 200 ℃ for 1h after mixing uniformly, soaking a sample cooled to room temperature into boiling water at 95 ℃ for 24h to remove the sodium chloride particles, and finally drying at 100 ℃ to obtain the nano-composite material.
The scanning electron microscope of the obtained material is shown in figure 1a, and the water contact angle of the material is shown in figure 1 b. From FIG. 1a, it can be seen that the material is a three-dimensionally connected porous structure; the contact angle of the prepared material with water is 146.8 degrees measured in figure 1 b; it can be seen from FIGS. 1b and 1c that the material prepared in example 1 has good hydrophobic and lipophilic properties.
FIG. 2a is an optical photograph of the material prepared in example 1 adsorbed to a magnet; FIG. 2b is a hysteresis chart of the prepared material (PDMS/ZFO); fig. 2 shows that the material prepared in example 1 has superparamagnetism and can be driven by magnetic force.
FIGS. 3a and 3b record the combustion of a commercially available polyurethane sponge (PU) and the material prepared in example 1 (PDMS-ZFO), respectively, during combustion for different times; FIG. 3c is a graph showing the heat release rate of a commercially available polyurethane sponge (PU) and the material prepared in example 1, and it can be seen that the peak value of the porous silicone rubber material (PDMS-ZFO) is significantly lower than that of the commercially available polyurethane sponge (PU), and the ignition time is delayed by a certain time; fig. 3d shows the mass residual percentage of the commercially available polyurethane sponge (PU) and the material prepared in example 1, and it can be seen that the carbon residual amount of the material prepared in example 1 is significantly higher than that of the commercially available polyurethane sponge, and the dense carbon layer helps to reduce the heat conduction to the inside, thereby achieving the flame retardant effect. Figure 3 illustrates the good fire resistance of the material prepared in example 1 compared to a common commercially available polyurethane sponge.
Fig. 4 is an optical photograph of the magnetic fire-resistant oil-absorbing porous silicone rubber material prepared in example 1 after being soaked in 2M sodium hydroxide (left in fig. 3), 2M hydrochloric acid (in fig. 3) and a saturated sodium chloride solution (right in fig. 3), respectively, for 2 hours. Figure 4 shows that the material prepared in example 1 has good chemical stability.
In fig. 5, a, b and c are optical photographs of the magnetic fireproof oil-absorbing porous silicone rubber material prepared in example 1 immersed in ethanol, acetone and dimethyl sulfoxide solvents respectively; e. f and g are the cycle curves of the material prepared in example 1 after being soaked in ethanol, acetone and dimethyl sulfoxide solvent for 3 hours, dried and compressed for 100 times, and the curves are tested by recording the compression distance after different forces are loaded. The sudden rise in stress after the compression to 55% in the figure is due to the fact that three-dimensionally connected skeletons collide with each other after the compression by a certain distance to cause sudden changes in stress. Figure 5 shows that the prepared material has good chemical and mechanical stability.
FIG. 6, a is an optical photograph of a tensile test of the magnetic fire-resistant oil-absorbing porous silicone rubber material prepared in example 1, and b is a curve of elongation at break of the material prepared in example 1, wherein the elongation at break is 45%, and the stress is 484 KPa, the curve being obtained by using a material equipped with a 500N load cell at room temperatureThe experiment was carried out in a universal tester for sensors (GOTECH TCS-2000, Taiwan, China) and then at 20 mm min-1The loading speed of (2) was tested. Fig. 6 shows that the material prepared has good mechanical properties.
Example 2
A preparation method of a magnetic fireproof oil-absorption porous silicon rubber material comprises the following steps:
(1) 20 mmol of Zn (NO)3)2·6H2O and 40 mmol of Fe (NO)3)3·9H2Dissolving O in distilled water, adjusting the pH value to 12 by using 5 mol/L sodium hydroxide, stirring for 2h in a water bath kettle at 70 ℃ to obtain a mixed solution, carrying out suction filtration on the mixed solution, washing for a plurality of times by using distilled water, drying for 1h in an oven at 50 ℃ to obtain a precursor, and finally calcining for 6h at 380 ℃ to obtain powdery Zinc Ferrite (ZFO) nanoparticles;
(2) adding 30g of sodium chloride particles and 0.45g of zinc ferrite nanoparticles into 4g of polydimethylsiloxane prepolymer, stirring and mixing uniformly, adding 0.36g of curing agent, then curing at 180 ℃ for 1.5h after mixing uniformly, soaking a sample cooled to room temperature into 80 ℃ boiling water for 12h to remove the sodium chloride particles, and finally drying at 90 ℃ to obtain the nano-zinc ferrite.
Example 3
A preparation method of a magnetic fireproof oil-absorption porous silicon rubber material comprises the following steps:
(1) 20 mmol of Zn (NO)3)2·6H2O and 40 mmol of Fe (NO)3)3·9H2Dissolving O in distilled water, adjusting the pH value to 12 by using 5 mol/L sodium hydroxide, stirring for 3h in a water bath kettle at 80 ℃ to obtain a mixed solution, carrying out suction filtration on the mixed solution, washing for a plurality of times by using distilled water, drying for 2h in an oven at 60 ℃ to obtain a precursor, and finally calcining for 3h at 400 ℃ to obtain powdery Zinc Ferrite (ZFO) nanoparticles;
(2) adding 28g of sodium chloride particles and 0.42g of zinc ferrite nanoparticles into 4g of polydimethylsiloxane prepolymer, stirring and mixing uniformly, adding 0.35g of curing agent, then curing at 200 ℃ for 2h after mixing uniformly, soaking a sample cooled to room temperature into 80 ℃ boiling water for 24h to remove the sodium chloride particles, and finally drying at 80 ℃ to obtain the nano-zinc ferrite.
Example 4
A preparation method of a magnetic fireproof oil-absorption porous silicon rubber material comprises the following steps:
(1) 20 mmol of Zn (NO)3)2·6H2O and 40 mmol of Fe (NO)3)3·9H2Dissolving O in distilled water, adjusting the pH value to 12 by using 5 mol/L sodium hydroxide, stirring for 1h in a water bath kettle at 60 ℃ to obtain a mixed solution, carrying out suction filtration on the mixed solution, washing for a plurality of times by using distilled water, drying for 3h in an oven at 70 ℃ to obtain a precursor, and finally calcining for 4h at 420 ℃ to obtain powdery Zinc Ferrite (ZFO) nanoparticles;
(2) adding 25g of sodium chloride particles and 0.4g of zinc ferrite nanoparticles into 4g of polydimethylsiloxane prepolymer, stirring and mixing uniformly, adding 0.4g of curing agent, then curing at 220 ℃ for 2.5h after mixing uniformly, soaking a sample cooled to room temperature into boiling water at 95 ℃ for 36h to remove the sodium chloride particles, and finally drying at 100 ℃ to obtain the nano-zinc ferrite.
Example 5
A preparation method of a magnetic fireproof oil-absorption porous silicon rubber material comprises the following steps:
(1) 20 mmol of Zn (NO)3)2·6H2O and 40 mmol of Fe (NO)3)3·9H2Dissolving O in distilled water, adjusting the pH value to 12 by using 5 mol/L sodium hydroxide, stirring for 1h in a water bath kettle at 60 ℃ to obtain a mixed solution, carrying out suction filtration on the mixed solution, washing for a plurality of times by using distilled water, drying for 3h in an oven at 60 ℃ to obtain a precursor, and finally calcining for 5h at 400 ℃ to obtain powdery Zinc Ferrite (ZFO) nanoparticles;
(2) adding 20g of sodium chloride particles and 0.4g of zinc ferrite nanoparticles into 4g of polydimethylsiloxane prepolymer, stirring and mixing uniformly, adding 0.4g of curing agent, then curing at 200 ℃ for 3h after mixing uniformly, soaking a sample cooled to room temperature into boiling water at 95 ℃ for 24h to remove the sodium chloride particles, and finally drying at 80 ℃ to obtain the nano-zinc ferrite.
The samples obtained in examples 2 to 5 have comparable hydrophobicity, oil adsorption, magnetic properties, and fire resistance to those of the product obtained in example 1.
It is obvious that the above examples are only for illustrating the effectiveness and practicability of the preparation method, and are not limiting to the embodiment, such as sodium chloride, but can be changed into sugar and other different forms, and it is not necessary to be exhaustive for each example, and obvious changes or modifications are covered by the scope of the present invention.
Claims (6)
1. The magnetic fireproof oil-absorbing porous silicone rubber material is characterized by being prepared by the following steps:
(1) mixing and dissolving soluble salts of zinc and soluble salts of iron, adjusting pH to be alkaline, stirring and reacting at the temperature of 60-80 ℃ for 1-3h to obtain a mixed solution, carrying out suction filtration, washing and drying on the mixed solution to obtain a precursor, and finally calcining to obtain powdery zinc ferrite nano particles;
(2) uniformly dispersing sodium chloride and the zinc ferrite nanoparticles obtained in the step (1) into a prepolymer, adding a curing agent, curing, cooling to room temperature, soaking in hot water, and drying to obtain the magnetic fireproof oil-absorbing porous silicon rubber material;
the soluble salt of zinc in the step (1) is Zn (NO)3)2·6H2O, soluble salts of iron being Fe (NO)3)3·9H2O；
In the step (2), the prepolymer is polydimethylsiloxane; the curing agent is Dow Corning SYLGARD 184;
in the step (2), the mass ratio of the sodium chloride to the prepolymer is (5-9): 1;
in the step (2), the mass ratio of the zinc ferrite nano particles to the prepolymer is 1: (8-10);
in the step (2), the mass ratio of the curing agent to the prepolymer is 1: (10-12);
the curing time in the step (2) is 1-3h, and the curing temperature is 180-220 ℃.
2. The magnetic fire-resistant oil-absorbing porous silicon rubber material as claimed in claim 1, wherein the molar ratio of the soluble salt of zinc to the soluble salt of iron in step (1) is 1 (1-2); the drying time is 1-3h, the drying temperature is 50-70 ℃, the calcining time is 3-6h, and the calcining temperature is 380-.
3. The magnetic fire-resistant oil-absorbing porous silicon rubber material as claimed in claim 1, wherein the soaking temperature in the step (2) is 80-95 ℃ and the soaking time is 12-36 h; the drying temperature is 80-100 ℃.
4. A preparation method of a magnetic fireproof oil-absorption porous silicon rubber material is characterized by comprising the following steps:
(1) mixing and dissolving soluble salts of zinc and soluble salts of iron, adjusting pH to be alkaline, stirring and reacting at the temperature of 60-80 ℃ for 1-3h to obtain a mixed solution, carrying out suction filtration, washing and drying on the mixed solution to obtain a precursor, and finally calcining to obtain powdery zinc ferrite nano particles;
(2) uniformly dispersing sodium chloride and the zinc ferrite nanoparticles obtained in the step (1) into a prepolymer, adding a curing agent, curing, cooling to room temperature, soaking in hot water, and drying to obtain the magnetic fireproof oil-absorbing porous silicon rubber material;
the soluble salt of zinc in the step (1) is Zn (NO)3)2·6H2O, soluble salts of iron being Fe (NO)3)3·9H2O；
In the step (2), the prepolymer is polydimethylsiloxane; the curing agent is Dow Corning SYLGARD 184;
in the step (2), the mass ratio of the sodium chloride to the prepolymer is (5-9): 1; in the step (2), the mass ratio of the zinc ferrite nano particles to the prepolymer is 1: (8-10); in the step (2), the mass ratio of the curing agent to the prepolymer is 1: (10-12); in the step (2), the curing time is 1-3h, and the curing temperature is 180-220 ℃; the soaking temperature is 80-95 ℃, and the soaking time is 12-36 h; the drying temperature is 80-100 ℃.
5. The preparation method according to claim 4, wherein the molar ratio of the soluble salt of zinc to the soluble salt of iron in the step (1) is 1 (1-2); the drying time is 1-3h, the drying temperature is 50-70 ℃, the calcining time is 3-6h, and the calcining temperature is 380-.
6. Use of the magnetic fire-resistant oil-absorbing porous silicone rubber material of any one of claims 1 to 3 in the preparation of a fire-resistant oil-absorbing material.
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| WO2017015648A1 (en) * | 2015-07-23 | 2017-01-26 | Ozkan Cengiz S | Magnetic hydrophobic porous graphene sponge for environmental and biological/medical applications |
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