CN113480857A - Controllable magnetic release microcapsule, preparation method, release control method and application thereof - Google Patents
Controllable magnetic release microcapsule, preparation method, release control method and application thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L91/00—Compositions of oils, fats or waxes; Compositions of derivatives thereof
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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
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L91/00—Compositions of oils, fats or waxes; Compositions of derivatives thereof
- C08L91/005—Drying oils
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L95/00—Compositions of bituminous materials, e.g. asphalt, tar, pitch
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/16—Halogen-containing compounds
- C08K2003/162—Calcium, strontium or barium halides, e.g. calcium, strontium or barium chloride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2275—Ferroso-ferric oxide (Fe3O4)
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
Abstract
The invention provides a controllable magnetic force release microcapsule, a preparation method, a release control method and application thereof. The microcapsule of the invention is added with magnetic powder, and the capsule wall can be broken by applying a magnetic field according to the road surface condition, so that the repair can be realized as required, thereby improving the utilization rate of the microcapsule and the road repair capability.
Description
Technical Field
The invention relates to the technical field of road repair materials, in particular to a controllable magnetic release microcapsule, a preparation method, a release control method and application thereof.
Background
The asphalt material is widely applied to road paving, the asphalt road is easy to form microcracks under the action of repeated vehicle load and temperature change, the microcracks gradually develop and are communicated with each other along with the increase of service time, and then large-size cracks are formed, so that the service life of the road is influenced. Particularly, the surface cracks of the asphalt roads can further aggravate the development of the cracks generated in rainfall, and the cracks which are not repaired in time are easy to develop into grooves or pits, so that the safety and the comfort of road driving are greatly influenced.
The cost of manpower and material resources consumed by the later maintenance of the asphalt road is high, and more attention is paid to preventive maintenance in recent years. The common preventive maintenance method is to mix the microcapsule encapsulated with the repairing agent into the asphalt mixture for road pavement. For the asphalt pavement containing the microcapsules, when the micro cracks are generated, the capsule shells at the corresponding positions are torn by the cracks, so that the repairing agent in the asphalt pavement is released, the self-repairing of the micro cracks is realized, the further derivation of the micro cracks is avoided, and the purpose of prolonging the service life of the pavement is achieved. It should be noted that the microcapsules may be activated only when the positions of the micro cracks are consistent with the positions of the microcapsules, but the distribution of the microcapsules and the positions of the micro cracks are random, so that the utilization rate of the microcapsules is limited, and the pavement crack repairing capability is limited.
Disclosure of Invention
The invention solves the problem of how to prepare a controllable release type microcapsule, which can realize active release under the action of external induction so as to improve the utilization rate of the microcapsule and the road repair capability.
In order to solve the problems, the invention provides a controllable magnetic force release microcapsule, which comprises a capsule wall and a capsule core, wherein the capsule wall wraps the capsule core, the capsule wall is made of calcium alginate, the capsule core is made of an asphalt repairing agent, and magnetic powder is distributed in the capsule wall and the capsule core.
Optionally, the mass fraction of the magnetic powder in the microcapsules is between 10 wt% and 40 wt%.
Optionally, the magnetic powder is selected from one or more of the following: neodymium iron boron, ferroferric oxide, manganese ferrite, zinc ferrite, nickel zinc ferrite, manganese magnesium zinc ferrite, magnetoplumbite and magnetic steel slag.
Optionally, the asphalt restoration agent is selected from one or more of: soybean oil, linseed oil, rape oil, rapeseed oil, castor oil, high oil, cottonseed oil, sunflower oil, palm oil, peanut oil, safflower oil, corn oil, animal fat and lecithin.
The second aspect of the present invention provides a method for preparing the above controllable magnetic force release microcapsule, comprising the following steps:
s1: adding the asphalt repairing agent into water, stirring and mixing to obtain liquid A;
s2: weighing sodium alginate and mixing with magnetic powder to obtain a solid mixture B, adding the solid mixture B into the liquid A, and stirring and mixing to obtain a liquid C;
s3: dropwise adding the liquid C into a calcium chloride solution, and stirring for reaction to obtain microcapsules;
s4: and (4) sieving the microcapsule prepared in the step S3, cleaning and drying.
Optionally, the volume of the mixed solution A in the step S1 is V1Wherein the volume ratio of the asphalt repairing agent to the water is between 1:5 and 1: 2.
Optionally, the total mass of the solid mixture B in the step S2 is M1Wherein the mass ratio of the magnetic powder to the sodium alginate is between 1:6 and 1: 1.
Alternatively, 2g to 3.33g of the mixed solid B is added per 100mL of the mixed solution a in the step S2.
Optionally, the mass fraction of the calcium chloride solution in the step S3 is between 1 wt% and 3 wt%.
The third aspect of the present invention provides a release control method for the above controllable magnetic force release microcapsule, comprising the following steps: applying a magnetic field to the microcapsule, wherein the magnetic field intensity is 1000G-10000G, the frequency is 5Hz-10Hz, and the application time is 1min-120 min.
The fourth aspect of the invention provides the application of the controllable magnetic force release microcapsule, and the controllable magnetic force release microcapsule is used in road asphalt pavement.
Compared with the prior art, the invention has the following beneficial effects:
the controllable magnetic force release microcapsule can actively control the release of the asphalt repairing agent of the capsule core, and the magnetic powder is added into the microcapsule, so that the capsule wall can be broken by applying a magnetic field according to the road surface condition, and the repair can be realized as required, thereby improving the utilization rate of the microcapsule and the road repairing capability.
The controllable magnetic force release microcapsule has the advantages of simple preparation method, controlled raw material consumption, ensured magnetic powder and repairing agent in proper amount, and specific material adding sequence, so that the prepared microcapsule has uniform particle size distribution, good stability, high mechanical strength, difficult breakage during road paving, high coating rate of the asphalt repairing agent and good pavement repairing effect.
The release control method of the controllable magnetic release microcapsule has the advantages of simple steps, good release effect, strong practicability and good application and popularization prospects.
Drawings
FIG. 1 is a flow chart of a method for preparing controlled magnetic release microcapsules in an embodiment of the present invention;
FIG. 2 is a graph showing the effect of the amount of magnetic powder added to the microcapsules on the amount of asphalt repair agent released in an experimental example of the present invention;
FIG. 3 is a graph showing the effect of the sodium alginate content in the microcapsules on the release amount of the asphalt repair agent in the experimental example of the present invention;
FIG. 4 is a graph showing a comparison of the influence of the magnetic field application time on the amount of asphalt repairing agent released in the experimental examples of the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below. It should be noted that the following examples are only used to illustrate the implementation method and typical parameters of the present invention, and are not used to limit the scope of the parameters of the present invention, so that reasonable variations can be made and still fall within the protection scope of the claims of the present invention.
It is noted that the endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and that such ranges or values are understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The embodiment of the invention discloses a controllable magnetic force release microcapsule, which comprises a capsule wall and a capsule core, wherein the capsule wall wraps the capsule core, the capsule wall is made of calcium alginate, the capsule core is made of an asphalt repairing agent, and magnetic powder is distributed in the capsule wall and the capsule core.
The microcapsule is a micro package with polymer wall, the grain diameter is 1mm-5mm, the capsule core is wrapped by the capsule wall, the asphalt repairing agent of the capsule core is isolated from the outside and can not be influenced by the environment, thereby keeping stability.
In the embodiment of the invention, the material of the capsule wall is calcium alginate, which has good thermal stability and mechanical strength, is not easy to break when paving roads, and avoids the asphalt repairing agent from releasing in advance.
In the embodiment of the present invention, the capsule core material is an asphalt repairing agent, most of small molecule oils can be used as the asphalt repairing agent, such as soybean oil, linseed oil, rape oil, rapeseed oil, castor oil, high oil, cottonseed oil, sunflower seed oil, palm oil, peanut oil, safflower oil, corn oil, animal fat, lecithin, etc., the asphalt repairing agent is selected from one small molecule oil or a mixture of multiple small molecule oils, and the asphalt repairing agent can be obtained by self-preparation or can be obtained commercially.
In the embodiment of the invention, the magnetic powder is distributed in the capsule wall and the capsule core of the microcapsule, the microcapsule is repeatedly extruded under the action of a circulating magnetic field, and the repairing agent is slowly released, so that the controllable release of the microcapsule is realized, the utilization rate of the microcapsule in a road surface is increased, and the self-repairing capability of the road is improved. The mass fraction of the magnetic powder in the microcapsule influences the controlled release effect, in the embodiment of the invention, the mass fraction of the magnetic powder in the controllable magnetic force release microcapsule is between 10 wt% and 40 wt%, and in this range, the microcapsule shows good controllability. The magnetic powder can be selected from any one of magnetic alloy powder, such as neodymium iron boron, ferroferric oxide, manganese ferrite, zinc ferrite, nickel zinc ferrite, manganese magnesium zinc ferrite, magnetoplumbite, magnetic steel slag and the like, and can also be formed by mixing various powders, and the magnetic powder can be prepared by self or obtained by commercial purchase. The magnetic properties of various magnetic powders are different, which affects the reaction of the microcapsule to the magnetic field, and when the magnetic field is applied to control the release of the microcapsule, the magnetic field parameters need to be adjusted according to the type and quality of the magnetic powder actually used to control the release effect of the microcapsule.
Another embodiment of the present invention discloses a method for preparing the above-mentioned controllable magnetic force release microcapsule, which is shown in fig. 1 and comprises the following steps:
s1: adding the asphalt repairing agent into water, stirring and mixing to obtain liquid A.
S2: weighing sodium alginate and mixing with magnetic powder to obtain a solid mixture B, adding the solid mixture B into the liquid A, and stirring and mixing to obtain a liquid C.
S3: and dropwise adding the liquid C into a calcium chloride solution, and stirring for reaction to obtain the microcapsule.
S4: and (4) sieving the microcapsule prepared in the step (S3), cleaning and drying.
The controllable magnetic release microcapsule is simple in preparation method, raw material materials are controlled, a proper amount of magnetic powder is guaranteed to be contained in the microcapsule, and a specific material adding sequence enables the prepared microcapsule to be uniform in particle size distribution, good in stability, high in mechanical strength, not prone to cracking during road paving, high in coating rate of an asphalt repairing agent, capable of releasing a large amount of asphalt repairing agent after capsule wall cracking, and good in pavement repairing effect.
According to a preferred embodiment of the present invention, the volume of the mixed solution A is V in step S11Wherein the volume ratio of the asphalt repairing agent to the water is between 1:5 and 1:2, so that the asphalt repairing agent can be uniformly dispersed in the water, the stirring speed is 100r/min to 500r/min, the stirring time is 0.5min to 5min, and the asphalt repairing agent in the liquid A is uniformly dispersed.
According to a preferred embodiment of the present invention, in step S2, the total mass of the solid mixture B is M1Wherein the mass ratio of the magnetic powder to the sodium alginate is between 1:6 and 1:1, 2g to 3.33g of the solid mixture B is added into each 100mL of the mixed solution A, the stirring is kept during the process of adding the solid mixture B into the liquid A, the stirring speed is kept between 100r/min and 500r/min, and the stirring is carried out for 5min to 15min, so as to obtain the uniform liquid C. According to a preferred embodiment of the present invention, in step S3, the mass fraction of calcium chloride is between 1 wt% and 3 wt%, the calcium chloride solution is kept in a stirring state during the dropping process to prevent the microcapsules from agglomerating, and the microcapsules can be prepared by stirring with an electromagnetic stirrer for a reaction time of 0.5h to 2 h.
According to a preferred embodiment of the present invention, in step S4, the microcapsules are screened and then washed with deionized water to ensure that the surface residues are cleaned, and then the microcapsules are placed into an oven, dried at 70-80 ℃ for 2-3 h, and then taken out and stored in an incubator at-20 ℃ for later use.
Another embodiment of the present invention discloses a release control method of the above controllable magnetic release microcapsule, comprising the steps of: a circulating magnetic field of a certain frequency is applied to the microcapsules. This step may be performed using a strong magnet such as a neodymium iron boron magnet to apply the magnetic field, or may provide an electromagnetic field to control the release of the microcapsules. This step allows the microcapsules to withstand repeated squeezing action, promoting the release of the healing agent. The release control method has the advantages of simple steps, good release effect, strong practicability and good application and popularization prospects.
According to a preferred embodiment of the invention, the magnetic field strength is 1000G to 10000G, the frequency is 5Hz to 10Hz, and the application time is 1min to 120 min. The magnetic field intensity, the frequency and the application time all have influence on the release amount of the microcapsules, the test surface can obtain better release effect within the parameter range, and the magnetic field parameters can be adjusted according to the release condition of the microcapsules in the actual use process.
The invention also discloses application of the controllable magnetic force release microcapsule in road asphalt. The controllable magnetic release microcapsule provided by the embodiment of the invention can be added into a road asphalt mixture and then used for road asphalt paving. When the asphalt road generates microcracks, a magnetic field is applied to the controllable magnetic force release microcapsules, so that the microcapsules can generate stimulation, an asphalt repairing agent is released, and the self repair of the road is accelerated. The controllable magnetic force release microcapsule can be actively released in a magnetic field applying mode due to the addition of the magnetic powder, so that the utilization rate of the microcapsule is improved, the pavement repair effect is improved, and the maintenance cost of the pavement is reduced.
The present invention will be described in detail below by way of specific examples.
Example 1
The following were prepared: 100ml sunflower oil, 500ml water, 0.2g neodymium iron boron powder, 0.8g sodium alginate, 1.2g calcium chloride dissolved in 60ml water to make 2% wt calcium chloride solution.
S1: adding sunflower seed oil into water, stirring and mixing at the rotation speed of 300r/min for 1min to obtain liquid A.
S2: and adding a solid mixture B of sodium alginate and neodymium iron boron powder into the liquid A, stirring and mixing, wherein the stirring speed is 300r/min, and the stirring time is 10min, so as to obtain a liquid C.
S3: and (3) placing the calcium chloride solution on an electromagnetic stirrer, dripping the liquid B into the calcium chloride solution in a constant-pressure separating funnel titration mode, and stirring for reacting for 1h to obtain the microcapsule.
S4: sieving the microcapsule, washing with deionized water to ensure that residual substances on the surface are cleaned, putting into an oven, drying at 80 deg.C for 2h, taking out to obtain the microcapsule with controllable magnetic force release, and storing in a-20 deg.C incubator.
Example 2
The following were prepared: 100ml sunflower oil, 500ml water, 0.4g neodymium iron boron powder, 0.8g sodium alginate, 1.2g calcium chloride dissolved in 60ml water to make 2% wt calcium chloride solution.
S1: adding sunflower seed oil into water, stirring and mixing at the rotation speed of 300r/min for 1min to obtain liquid A.
S2: and adding a solid mixture B of sodium alginate and neodymium iron boron powder into the liquid A, stirring and mixing, wherein the stirring speed is 300r/min, and the stirring time is 10min, so as to obtain a liquid C.
S3: and (3) placing the calcium chloride solution on an electromagnetic stirrer, dripping the liquid B into the calcium chloride solution in a constant-pressure separating funnel titration mode, and stirring for reacting for 1h to obtain the microcapsule.
S4: sieving the microcapsule, washing with deionized water to ensure that residual substances on the surface are cleaned, putting into an oven, drying at 80 deg.C for 2h, taking out to obtain the microcapsule with controllable magnetic force release, and storing in a-20 deg.C incubator.
Example 3
The following were prepared: 100ml sunflower oil, 500ml water, 0.4g neodymium iron boron powder, 1.2g sodium alginate, 1.2g calcium chloride dissolved in 60ml water to make 2% wt calcium chloride solution.
S1: adding sunflower seed oil into water, stirring and mixing at the rotation speed of 300r/min for 1min to obtain liquid A.
S2: and adding a solid mixture B of sodium alginate and neodymium iron boron powder into the liquid A, stirring and mixing, wherein the stirring speed is 300r/min, and the stirring time is 10min, so as to obtain a liquid C.
S3: and (3) placing the calcium chloride solution on an electromagnetic stirrer, dripping the liquid B into the calcium chloride solution in a constant-pressure separating funnel titration mode, and stirring for reacting for 1h to obtain the microcapsule.
S4: sieving the microcapsule, washing with deionized water to ensure that residual substances on the surface are cleaned, putting into an oven, drying at 80 deg.C for 2h, taking out to obtain the microcapsule with controllable magnetic force release, and storing in a-20 deg.C incubator.
Example 4
The following were prepared: 100ml sunflower oil, 500ml water, 0.3g neodymium iron boron powder, 0.8g sodium alginate, 1.2g calcium chloride dissolved in 60ml water to make 2% wt calcium chloride solution.
S1: adding sunflower seed oil into water, stirring and mixing at the rotation speed of 300r/min for 1min to obtain liquid A.
S2: and adding a solid mixture B of sodium alginate and neodymium iron boron powder into the liquid A, stirring and mixing, wherein the stirring speed is 300r/min, and the stirring time is 10min, so as to obtain a liquid C.
S3: and (3) placing the calcium chloride solution on an electromagnetic stirrer, dripping the liquid B into the calcium chloride solution in a constant-pressure separating funnel titration mode, and stirring for reacting for 1h to obtain the microcapsule.
S4: sieving the microcapsule, washing with deionized water to ensure that residual substances on the surface are cleaned, putting into an oven, drying at 80 deg.C for 2h, taking out to obtain the microcapsule with controllable magnetic force release, and storing in a-20 deg.C incubator.
Example 5
The following were prepared: 100ml sunflower oil, 500ml water, 0.4g neodymium iron boron powder, 1g sodium alginate, 1.2g calcium chloride dissolved in 60ml water to make 2% wt calcium chloride solution.
S1: adding sunflower seed oil into water, stirring and mixing at the rotation speed of 300r/min for 1min to obtain liquid A.
S2: and adding a solid mixture B of sodium alginate and neodymium iron boron powder into the liquid A, stirring and mixing, wherein the stirring speed is 300r/min, and the stirring time is 10min, so as to obtain a liquid C.
S3: and (3) placing the calcium chloride solution on an electromagnetic stirrer, dripping the liquid B into the calcium chloride solution in a constant-pressure separating funnel titration mode, and stirring for reacting for 1h to obtain the microcapsule.
S4: sieving the microcapsule, washing with deionized water to ensure that residual substances on the surface are cleaned, putting into an oven, drying at 80 deg.C for 2h, taking out to obtain the microcapsule with controllable magnetic force release, and storing in a-20 deg.C incubator.
Example 6
The following were prepared: 200ml of linseed oil, 400ml of water, 0.3g of ferroferric oxide powder, 0.6g of sodium alginate and 1.8g of calcium chloride are dissolved in 60ml of water to prepare a 3 wt% calcium chloride solution.
S1: adding linseed oil into water, stirring and mixing at a stirring speed of 500r/min for 3min to obtain liquid A.
S2: and adding a solid mixture B of sodium alginate and ferroferric oxide into the liquid A, stirring and mixing, wherein the stirring speed is 500r/min, and the stirring time is 15min, so as to obtain liquid C.
S3: and (3) placing the calcium chloride solution on an electromagnetic stirrer, dripping the liquid B into the calcium chloride solution in a constant-pressure separating funnel titration mode, and stirring for reacting for 2 hours to obtain the microcapsule.
S4: sieving the microcapsule, washing with deionized water to ensure that residual substances on the surface are cleaned, putting into an oven, drying at 90 deg.C for 3h, taking out to obtain the microcapsule with controllable magnetic force release, and storing in a-20 deg.C incubator.
Example 7
The following were prepared: 150ml of animal fat, 450ml of water, 0.5g of manganese ferrite powder, 1g of sodium alginate and 0.6g of calcium chloride are dissolved in 60ml of water to prepare a 1% wt calcium chloride solution.
S1: adding animal fat into water, stirring and mixing at a stirring speed of 400r/min for 2min to obtain liquid A.
S2: and adding a solid mixture B of sodium alginate and manganese ferrite into the liquid A, stirring and mixing, wherein the stirring speed is 500r/min, and the stirring time is 5min to obtain a liquid C.
S3: and (3) placing the calcium chloride solution on an electromagnetic stirrer, dripping the liquid B into the calcium chloride solution in a constant-pressure separating funnel titration mode, and stirring for reacting for 1.5h to obtain the microcapsule.
S4: sieving the microcapsule, washing with deionized water to ensure that residual substances on the surface are cleaned, putting into an oven, drying at 70 deg.C for 2.5h, taking out to obtain the microcapsule with controllable magnetic force release, and storing in an incubator at-20 deg.C.
Example 8
The following were prepared: 50ml of soybean oil, 50ml of rape oil, 30ml of rapeseed oil, 460ml of water, 0.2g of magnetoplumbite powder, 0.2g of magnetic steel slag powder, 0.7g of sodium alginate and 1.2g of calcium chloride are dissolved in 60ml of water to prepare a 2 wt% calcium chloride solution.
S1: adding soybean oil, rape oil and rapeseed oil into water, stirring and mixing, wherein the stirring speed is 100r/min, and the stirring time is 5min, so as to obtain a liquid A.
S2: and adding a solid mixture B of sodium alginate, magnetoplumbite and magnetic steel slag into the liquid A, stirring and mixing, wherein the stirring speed is 100r/min, and the stirring time is 15min, so as to obtain a liquid C.
S3: and (3) placing the calcium chloride solution on an electromagnetic stirrer, dripping the liquid B into the calcium chloride solution in a constant-pressure separating funnel titration mode, and stirring for reacting for 0.5h to obtain the microcapsule.
S4: sieving the microcapsule, washing with deionized water to ensure that residual substances on the surface are cleaned, putting into an oven, drying at 70 deg.C for 2h, taking out to obtain the microcapsule with controllable magnetic force release, and storing in a-20 deg.C incubator.
Example 9
The following were prepared: 200ml castor oil, 200ml high oil, 800ml water, 1.5g manganese magnesium zinc ferrite powder, 2g sodium alginate, 1.8g calcium chloride dissolved in 120ml water to make 1.5% wt calcium chloride solution.
S1: adding castor oil and high-oil soybean oil into water, stirring and mixing, wherein the stirring speed is 450r/min, and the stirring time is 4min to obtain liquid A.
S2: and adding a solid mixture B of sodium alginate and manganese-magnesium-zinc ferrite into the liquid A, stirring and mixing, wherein the stirring speed is 350r/min, and the stirring time is 12min to obtain a liquid C.
S3: and (3) placing the calcium chloride solution on an electromagnetic stirrer, dripping the liquid B into the calcium chloride solution in a constant-pressure separating funnel titration mode, and stirring for reacting for 1.5h to obtain the microcapsule.
S4: sieving the microcapsule, washing with deionized water to ensure that residual substances on the surface are cleaned, putting into an oven, drying at 90 deg.C for 3h, taking out to obtain the microcapsule with controllable magnetic force release, and storing in a-20 deg.C incubator.
Example 10
The following were prepared: 140ml cottonseed oil, 420ml water, 0.5g neodymium iron boron powder, 0.7g sodium alginate, 1.2g calcium chloride in 60ml water to make a 2% wt calcium chloride solution.
S1: adding the cottonseed oil into water, stirring and mixing, wherein the stirring speed is 500r/min, and the stirring time is 0.5min, so as to obtain liquid A.
S2: and adding the solid mixture B of sodium alginate and neodymium iron boron into the liquid A, stirring and mixing at the stirring speed of 500r/min for 5min to obtain liquid C.
S3: and (3) placing the calcium chloride solution on an electromagnetic stirrer, dripping the liquid B into the calcium chloride solution in a constant-pressure separating funnel titration mode, and stirring for reacting for 1h to obtain the microcapsule.
S4: sieving the microcapsule, washing with deionized water to ensure that residual substances on the surface are cleaned, putting into an oven, drying for 2h at 80 ℃, taking out to obtain the microcapsule with controllable magnetic force release, and storing in a heat preservation box at-20 ℃.
Example 11
The following were prepared: 160ml of palm oil, 480ml of water, 0.2g of neodymium iron boron powder, 0.3g of ferroferric oxide powder, 0.8g of sodium alginate and 1.2g of calcium chloride are dissolved in 60ml of water to prepare a 2 wt% calcium chloride solution.
S1: adding palm oil into water, stirring and mixing, wherein the stirring speed is 200r/min, and the stirring time is 2min, so as to obtain liquid A.
S2: and adding mixed powder B of sodium alginate, neodymium iron boron and ferroferric oxide into the liquid A, stirring and mixing, wherein the stirring speed is 150r/min, and the stirring time is 8min, so as to obtain liquid C.
S3: and (3) placing the calcium chloride solution on an electromagnetic stirrer, dripping the liquid B into the calcium chloride solution in a constant-pressure separating funnel titration mode, and stirring for reacting for 2 hours to obtain the microcapsule.
S4: sieving the microcapsule, washing with deionized water to ensure that residual substances on the surface are cleaned, putting into an oven, drying at 80 deg.C for 2h, taking out to obtain the microcapsule with controllable magnetic force release, and storing in a-20 deg.C incubator.
Example 12
The following were prepared: 150ml of peanut oil, 50ml of corn oil, 500ml of water, 1g of manganese ferrite powder, 1.2g of sodium alginate and 1.2g of calcium chloride are dissolved in 60ml of water to obtain a 2% wt calcium chloride solution.
S1: adding peanut oil and corn oil into water, stirring and mixing, wherein the stirring speed is 360r/min, and the stirring time is 3min, so as to obtain liquid A.
S2: and adding a solid mixture B of sodium alginate and manganese ferrite into the liquid A, stirring and mixing, wherein the stirring speed is 360r/min, and the stirring time is 6min, so as to obtain a liquid C.
S3: and (3) placing the calcium chloride solution on an electromagnetic stirrer, dripping the liquid B into the calcium chloride solution in a constant-pressure separating funnel titration mode, and stirring for reacting for 1h to obtain the microcapsule.
S4: sieving the microcapsule, washing with deionized water to ensure that residual substances on the surface are cleaned, putting into an oven, drying at 80 deg.C for 2h, taking out to obtain the microcapsule with controllable magnetic force release, and storing in a-20 deg.C incubator.
Example 13
The following were prepared: 70ml of safflower oil, 80ml of sunflower oil, 400ml of water, 0.8g of zinc ferrite powder, 0.8g of sodium alginate and 1.2g of calcium chloride are dissolved in 60ml of water to prepare a 2% wt calcium chloride solution.
S1: adding safflower oil and sunflower seed oil into water, stirring and mixing at a stirring speed of 200r/min for 5min to obtain liquid A.
S2: and adding a solid mixture B of sodium alginate and zinc ferrite into the liquid A, stirring and mixing, wherein the stirring speed is 300r/min, and the stirring time is 13min to obtain a liquid C.
S3: and (3) placing the calcium chloride solution on an electromagnetic stirrer, dripping the liquid B into the calcium chloride solution in a constant-pressure separating funnel titration mode, and stirring for reacting for 2 hours to obtain the microcapsule.
S4: sieving the microcapsule, washing with deionized water to ensure that residual substances on the surface are cleaned, putting into an oven, drying at 80 deg.C for 2h, taking out to obtain the microcapsule with controllable magnetic force release, and storing in a-20 deg.C incubator.
Example 14
The following were prepared: 160ml of lecithin, 440ml of water, 0.2g of zinc ferrite powder, 0.6g of nickel zinc ferrite powder, 1.4g of sodium alginate and 1.6g of calcium chloride are dissolved in 80ml of water to prepare a 2% wt calcium chloride solution.
S1: adding lecithin into water, stirring and mixing, wherein the stirring speed is 460r/min, and the stirring time is 4min, so as to obtain liquid A.
S2: and adding a solid mixture B of sodium alginate, zinc ferrite and nickel zinc ferrite into the liquid A, stirring and mixing, wherein the stirring speed is 480r/min, and the stirring time is 10min to obtain a liquid C.
S3: and (3) placing the calcium chloride solution on an electromagnetic stirrer, dripping the liquid B into the calcium chloride solution in a constant-pressure separating funnel titration mode, and stirring for reacting for 1.5h to obtain the microcapsule.
S4: sieving the microcapsule, washing with deionized water to ensure that residual substances on the surface are cleaned, putting into an oven, drying at 80 deg.C for 2h, taking out to obtain the microcapsule with controllable magnetic force release, and storing in a-20 deg.C incubator.
Example 15
The following were prepared: 20ml of soybean oil, 20ml of linseed oil, 20ml of rape oil, 20ml of rapeseed oil, 500ml of water, 0.1g of neodymium iron boron powder, 0.1g of ferroferric oxide powder, 0.1g of manganese ferrite powder, 1g of sodium alginate and 1.2g of calcium chloride are dissolved in 60ml of water to prepare a 2 wt% calcium chloride solution.
S1: adding soybean oil, linseed oil, rape oil and rapeseed oil into water, stirring and mixing, wherein the stirring speed is 300r/min, and the stirring time is 2min, so as to obtain liquid A.
S2: and adding a solid mixture B of sodium alginate, neodymium iron boron, ferroferric oxide and manganese ferrite into the liquid A, stirring and mixing, wherein the stirring speed is 300r/min, and the stirring time is 10min to obtain liquid C.
S3: and (3) placing the calcium chloride solution on an electromagnetic stirrer, dripping the liquid B into the calcium chloride solution in a constant-pressure separating funnel titration mode, and stirring for reacting for 0.5h to obtain the microcapsule.
S4: sieving the microcapsule, washing with deionized water to ensure that residual substances on the surface are cleaned, putting into an oven, drying at 80 deg.C for 2h, taking out to obtain the microcapsule with controllable magnetic force release, and storing in a-20 deg.C incubator.
Examples of the experiments
Experimental examples were set to test the release conditions of the microcapsules prepared in the above examples, and experimental groups and control groups were set, wherein a circulating magnetic field was applied to the experimental groups with a strong magnet, the amplitude of the magnetic field was 1000G to 1800G, the frequency of the magnetic field was 5Hz to 6Hz, and no magnetic field was applied to the control groups. And placing the capsule in a tetrafluoroethylene container to receive a circulating magnetic field, taking out the capsule after the testing time is up, flushing the tetrafluoroethylene container by using hexane, and testing the concentration of the repairing agent in the flushing liquid by using an ultraviolet-visible light spectrophotometer to represent the release amount of the capsule.
Experimental example 1
3 of the controlled-magnetic-force-releasing microcapsules prepared in example 1 were selected as an experimental group to which a magnetic field was applied, and the other 3 of the controlled-magnetic-force-releasing microcapsules prepared in example 1 were selected as a control group to which no magnetic field was applied. After 1h, the average release amount of the asphalt repairing agent of the experimental group is measured to be 0.0018g, and the average release amount of the asphalt repairing agent of the control group is measured to be 0.0012 g.
Experimental example 2
3 of the microcapsules with controllable magnetic release obtained in example 2 were selected as the experimental group to which a magnetic field was applied, and the other 3 of the microcapsules with controllable magnetic release obtained in example 2 were selected as the control group to which no magnetic field was applied. After 1h, the average release amount of the asphalt repairing agent in the experimental group is measured to be 0.0015g, and the average release amount of the asphalt repairing agent in the control group is measured to be 0.0003 g.
Experimental example 3
5 of the controlled-magnetic-force-releasing microcapsules prepared in example 3 were selected as an experimental group to which a magnetic field was applied, and the other 5 of the controlled-magnetic-force-releasing microcapsules prepared in example 3 were selected as a control group to which no magnetic field was applied. After 1h, the average release amount of the asphalt repairing agent of the experimental group is measured to be 0.0032g, and the average release amount of the asphalt repairing agent of the control group is measured to be 0.0020 g.
Experimental example 4
6 of the controlled-magnetic-force-releasing microcapsules prepared in example 4 were selected as an experimental group to which a magnetic field was applied, and the other 6 of the controlled-magnetic-force-releasing microcapsules prepared in example 4 were selected as a control group to which no magnetic field was applied. After 1h, the average release amount of the asphalt repair agent of the experimental group is measured to be 0.0017g, and the average release amount of the asphalt repair agent of the control group is measured to be 0.0009 g.
Experimental example 5
5 of the controlled-magnetic-force-releasing microcapsules prepared in example 5 were selected as an experimental group to which a magnetic field was applied, and the other 5 of the controlled-magnetic-force-releasing microcapsules prepared in example 5 were selected as a control group to which no magnetic field was applied. After 1h, the average release amount of the asphalt repairing agent of the experimental group is measured to be 0.0031g, and the average release amount of the asphalt repairing agent of the control group is measured to be 0.0019 g.
Experimental example 6
4 of the microcapsules with controllable magnetic force release prepared in example 2 were selected as the experimental group to which a magnetic field was applied, and the other 4 of the microcapsules with controllable magnetic force release prepared in example 2 were selected as the control group to which no magnetic field was applied. After 0.5h, the average release amount of the asphalt repair agent of the experimental group is measured to be 0.0011g, and the average release amount of the asphalt repair agent of the control group is 0.0010 g.
Experimental example 7
4 of the microcapsules with controllable magnetic force release prepared in example 2 were selected as the experimental group to which a magnetic field was applied, and the other 4 of the microcapsules with controllable magnetic force release prepared in example 2 were selected as the control group to which no magnetic field was applied. After 2h, the average release amount of the asphalt repair agent of the experimental group is measured to be 0.0061g, and the average release amount of the asphalt repair agent of the control group is measured to be 0.0013 g.
The results of the above experimental examples 1 to 7 show that the release amount of the asphalt repair agent is significantly increased after the magnetic field is applied to the controllable magnetic release microcapsules, so that the release of the controllable magnetic release microcapsules in the embodiments of the present invention can be actively controlled by applying the magnetic field, thereby increasing the utilization rate of the microcapsules and improving the road repair effect.
In addition, the results of experimental examples 1, 2 and 4 were compared to analyze the influence of the content of the magnetic powder on the release amount of the controlled magnetic force releasing microcapsules, and the comparison results are shown in fig. 2.
The influence of the sodium alginate content on the release amount of the controllable magnetic force release microcapsules can be analyzed by comparing the results of experimental example 2, experimental example 3 and experimental example 5, and the comparison result is shown in fig. 3.
The results of experimental example 2, experimental example 6 and experimental example 7 were compared to analyze the effect of the magnetic field acting time on the release amount of the controllable magnetic force release microcapsules, and the comparison results are shown in fig. 4.
Although the present invention is disclosed above, the present invention is not limited thereto. Various changes and modifications may be effected therein by one skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. The controllable magnetic release microcapsule is characterized by comprising a capsule wall and a capsule core, wherein the capsule wall wraps the capsule core, the capsule wall is made of calcium alginate, the capsule core is made of an asphalt repairing agent, and magnetic powder is distributed in the capsule wall and the capsule core.
2. The controlled magnetic release microcapsule of claim 1, wherein the mass fraction of said magnetic powder in said microcapsule is between 10% and 40% by weight.
3. A controlled magnetic release microcapsule according to claim 1 or 2, wherein said magnetic powder is selected from one or more of the following: neodymium iron boron, ferroferric oxide, manganese ferrite, zinc ferrite, nickel zinc ferrite, manganese magnesium zinc ferrite, magnetoplumbite and magnetic steel slag.
4. A controlled magnetic release microcapsule according to claim 1 or 2, characterized in that the bitumen repair agent is selected from one or more of: soybean oil, linseed oil, rape oil, rapeseed oil, castor oil, high oil, cottonseed oil, sunflower oil, palm oil, peanut oil, safflower oil, corn oil, animal fat and lecithin.
5. A process for the preparation of controlled magnetic release microcapsules according to any of claims 1 to 4, comprising the steps of:
s1: adding the asphalt repairing agent into water, stirring and mixing to obtain liquid A;
s2: weighing sodium alginate and mixing with magnetic powder to obtain a solid mixture B, adding the solid mixture B into the liquid A, and stirring and mixing to obtain a liquid C;
s3: dropwise adding the liquid C into a calcium chloride solution, and stirring for reaction to obtain microcapsules;
s4: and (4) sieving the microcapsule prepared in the step S3, cleaning and drying.
6. The method for preparing controlled magnetic release microcapsules of claim 5, wherein the volume of said mixed solution A in step S1 is V1Wherein the volume ratio of the asphalt repairing agent to the water is between 1:5 and 1: 2.
7. The method for preparing controlled magnetic release microcapsules of claim 5, wherein the total mass of said solid mixture B in step S2 is M1Wherein the mass ratio of the magnetic powder to the sodium alginate is between 1:6 and 1: 1.
8. The method for preparing controlled-release microcapsules according to claim 5, wherein 2g to 3.33g of said mixed solid B is added to 100mL of said mixed solution A in said step S2.
9. A method for controlling the release of controlled magnetic release microcapsules according to any of claims 1 to 4, comprising the steps of: applying a magnetic field to the microcapsule, wherein the magnetic field intensity is 1000G-10000G, the frequency is 5Hz-10Hz, and the application time is 1min-120 min.
10. Use of the controllable magnetic force release microcapsules according to any one of claims 1 to 4, wherein the controllable magnetic force release microcapsules are used in asphalt road surfacing.
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