CN113083040B - Preparation method of soot carbon-based composite membrane material - Google Patents
Preparation method of soot carbon-based composite membrane material Download PDFInfo
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- CN113083040B CN113083040B CN202110439608.4A CN202110439608A CN113083040B CN 113083040 B CN113083040 B CN 113083040B CN 202110439608 A CN202110439608 A CN 202110439608A CN 113083040 B CN113083040 B CN 113083040B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/38—Polyalkenylalcohols; Polyalkenylesters; Polyalkenylethers; Polyalkenylaldehydes; Polyalkenylketones; Polyalkenylacetals; Polyalkenylketals
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- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
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Abstract
A preparation method of a soot carbon-based composite membrane material comprises the following steps: preparing a film forming solution, wherein the film forming solution comprises a granular film forming matrix and a net forming agent, and the net forming agent can enable the film forming matrix to form a three-dimensional network structure; preparing a curing agent, wherein the curing agent is used for forming a composite film material with the three-dimensional network structure through a net forming agent in the film forming liquid when the film forming liquid is contacted with the curing agent; preparing a composite membrane material, namely dropwise adding the membrane forming solution on the curing agent, separating out liquid in the membrane forming solution by using the curing agent, and curing the membrane forming matrix to form the composite membrane material with the three-dimensional network structure; wherein the curing agent is sodium chloride, and the mass ratio of the sodium chloride to the net forming agent in the film forming liquid is not less than 10: 1.
Description
Technical Field
The invention belongs to the technical field of new materials, and particularly relates to a preparation technology of a soot carbon-based composite membrane material.
Background
Soot carbon is an aggregate of carbon particles, mainly derived from automobile exhaust and by-products of combustion processes of fossil fuels, candles, biomass, etc., and is considered to be a pollutant harmful to the environment and human health. However, due to the advantages of abundant sources, simple preparation process, high temperature resistance and the like, the functional material is widely concerned at present.
The soot carbon particles have small diameter, low density, black powder appearance and chemical inertness, so that the soot carbon particles are connected with each other to form a three-dimensional network to prepare a processable soot carbon-based block or film material, which becomes a bottleneck problem limiting the application of the soot carbon-based block or film material.
Disclosure of Invention
The invention aims to provide a preparation method of a soot carbon-based composite film material.
The invention relates to a preparation method of a soot carbon-based composite membrane material, which comprises the following steps:
step (1): preparing a film forming solution, wherein the film forming solution comprises a granular film forming matrix and a net forming agent, and the net forming agent can enable the film forming matrix to form a three-dimensional network structure;
step (2): preparing a curing agent, wherein the curing agent is used for forming the composite membrane material with the three-dimensional network structure through a web forming agent in the film forming solution when the film forming solution is contacted with the curing agent;
and (3): preparing a composite membrane material, dripping the film-forming solution on the curing agent, separating out the liquid in the film-forming solution by the curing agent, and curing the film-forming substrate to form the composite membrane material with the three-dimensional network structure;
wherein the curing agent is sodium chloride, and the mass ratio of the sodium chloride to the net forming agent in the film forming liquid is not less than 10: 1.
the invention has the advantages that: the method is simple and easy to operate, extremely mild in reaction conditions, green and pollution-free, and has amplification potential; and composite membrane materials with different pore structures can be obtained by adjusting the granular film forming matrix and the web forming agent.
Drawings
Fig. 1 is a schematic flow chart of a preparation method of a soot carbon-based composite film material provided in an example of the present application, fig. 2 is a real object diagram of a composite film material SP-1 prepared by a preparation method provided in example 1, fig. 3 is an SEM diagram of the composite film material SP-1 prepared by the preparation method provided in example 1, fig. 4 is an SEM diagram of a composite film material SP-2 prepared by the preparation method provided in example 2, fig. 5 is an SEM diagram of a composite film material SP-3 prepared by the preparation method provided in example 3, and fig. 6 is a schematic diagram of surface moisture evaporation amount and corresponding photothermal conversion efficiency of the composite film materials SP-1, SP-2 and SP-3 prepared in example 1, example 2 and example 3 under a simulated solar light irradiation intensity of 1 kW m-2.
Detailed Description
The invention relates to a preparation method of a soot carbon-based composite membrane material, which comprises the following steps:
preparing a film forming solution, wherein the film forming solution comprises a granular film forming matrix and a net forming agent, and the net forming agent can enable the film forming matrix to form a three-dimensional network structure;
preparing a curing agent, wherein the curing agent is used for forming a composite film material with the three-dimensional network structure through a net forming agent in the film forming liquid when the film forming liquid is contacted with the curing agent;
preparing a composite membrane material, namely dropwise adding the membrane forming solution on the curing agent, separating out liquid in the membrane forming solution by using the curing agent, and curing the membrane forming matrix to form the composite membrane material with the three-dimensional network structure;
wherein the curing agent is sodium chloride, and the mass ratio of the sodium chloride to the net forming agent in the film forming liquid is not less than 10: 1.
in the preparation method, the web-forming agent in the step (1) is a polyvinyl alcohol aqueous solution, and the mass concentration of the polyvinyl alcohol aqueous solution is not less than 5%.
In the above preparation method, when the mass concentration of the sodium chloride in the step (3) is greater than the preset concentration, hydrogen bonds between water molecules and polyvinyl alcohol in the polyvinyl alcohol aqueous solution are reduced, and the polyvinyl alcohol aqueous solution is salted out; the polyvinyl alcohol chains are subjected to intermolecular aggregation and further serve as physical nodes to form the three-dimensional network structure in the film.
In the above preparation method, the film-forming substrate in step (1) is soot carbon, and the step of preparing the film-forming solution includes: and washing the soot carbon by using acetone and ethanol in sequence, drying at a preset temperature for a first preset time, and grinding to obtain the film-forming matrix. The preset temperature is 80-120 ℃, and the first preset time is 12-24 hours.
In the above preparation method, the mass ratio of the film-forming substrate to the web-forming agent in the film-forming solution in step (1) is 1:1 to 5.
According to the preparation method, the mass concentration of the film forming substrate in the step (1) in the film forming solution is 2.9-10.7%.
In the preparation method, the step of dripping the deposition solution on the curing agent in the step (3) comprises dripping the deposition solution on the curing agent, standing for a second preset time, soaking in distilled water, and freeze-drying to obtain the composite membrane material. The second preset time is 12-24 hours.
The present invention will be described in further detail with reference to the following examples and drawings.
The embodiment of the invention provides a preparation method of a soot carbon-based composite membrane material, and as shown in fig. 1, fig. 1 is a flow schematic diagram of the preparation method of the soot carbon-based composite membrane material provided by the embodiment of the application. The method comprises the following steps:
s101, preparing a film forming solution, wherein the film forming solution comprises a granular film forming matrix and a net forming agent, and the net forming agent can enable the film forming matrix to form a three-dimensional network structure;
s102, preparing a curing agent, wherein the curing agent is used for forming a composite membrane material with a three-dimensional network structure through a network forming agent in the film forming liquid when the film forming liquid is contacted with the curing agent;
s103, preparing a composite membrane material, dripping the film forming solution on a curing agent, precipitating the liquid in the film forming solution by the curing agent, and curing a film forming matrix to form the composite membrane material with a three-dimensional network structure;
wherein the curing agent is sodium chloride, and the mass ratio of the sodium chloride to the net forming agent in the film forming liquid is not less than 10: 1.
according to the method provided by the embodiment of the invention, based on the sodium chloride curing agent, when the net forming agent in the film forming solution is contacted with the sodium chloride, the mass ratio of the sodium chloride to the net forming agent is not less than 10:1, namely the content of the sodium chloride is far greater than that of the net forming agent, so that the liquid in the film forming solution can be precipitated, and the film forming substrate is cured to form the composite film material with a three-dimensional network structure. The method provided by the embodiment of the application is simple and easy to operate, extremely mild in reaction conditions, green and pollution-free, and has amplification potential; and composite membrane materials with different pore structures can be obtained by adjusting the granular film forming matrix and the web forming agent.
The methods provided by the embodiments of the present invention will be further explained and illustrated by the optional examples.
S101, preparing a film forming solution, wherein the film forming solution comprises a granular film forming matrix and a net forming agent, and the net forming agent can enable the film forming matrix to form a three-dimensional network structure.
In an alternative embodiment, the film-forming substrate is soot carbon, and the step of preparing the deposition solution comprises: and washing the soot carbon by using acetone and ethanol in sequence, drying the soot carbon for a first preset time at a preset temperature, and grinding the soot carbon to obtain a film-forming matrix.
The soot carbon provided by the embodiment of the application is a common carbon-based byproduct, belongs to waste recycling, and is rich in body source and low in cost.
In an optional embodiment, the predetermined temperature is 80 ℃ to 120 ℃, such as 100 ℃, 105 ℃, 110 ℃, 120 ℃, and the like. The first preset time is 12-24 hours. Such as 12 hours, 13 hours, 14 hours, 23 hours, 24 hours, etc.
In an optional embodiment, the mass ratio of the film forming substrate to the reticulating agent in the film forming solution is 1: 1-5. The amount of the network-forming agent in the film-forming solution should not be too large, which may result in failure to bond the film-forming substrate and increase the production cost. For example, the mass ratio of the film-forming substrate to the web-forming agent in the deposition solution may be 1:1, 1:2, 1:3, 1:4, 1:5, or the like.
In an alternative embodiment, the mass concentration of the film-forming substrate in the deposition solution is 2.9% to 10.7%.
In an alternative embodiment, the netting agent is an aqueous solution of polyvinyl alcohol, and the mass concentration of the aqueous solution of polyvinyl alcohol is not less than 5%.
S102, preparing a curing agent, wherein the curing agent is used for forming a composite membrane material with a three-dimensional network structure through a network forming agent in the film forming liquid when the film forming liquid is contacted with the curing agent.
The curing agent provided by the embodiment of the invention is sodium chloride, namely, the sodium chloride can be tabletted according to the requirement of a film material, namely, the thickness, size, shape and the like of the sodium chloride tabletted sheet can be selected according to the requirement, and the sodium chloride tabletted sheet is not limited in the embodiment of the application.
S103, preparing a composite membrane material, dripping the film forming solution on a curing agent, precipitating the liquid in the film forming solution by the curing agent, and curing a film forming matrix to form the composite membrane material with a three-dimensional network structure;
wherein the curing agent is sodium chloride, and the mass ratio of the sodium chloride to the net forming agent in the film forming liquid is not less than 10: 1.
in an alternative embodiment, the step of dropping the deposition solution on the curing agent comprises dropping the deposition solution on a sodium chloride press plate, standing for a second preset time, soaking in distilled water, and freeze-drying to obtain the composite membrane material.
In an optional embodiment, the second preset time is 12 hours to 24 hours. Illustratively, the resting time may be 12 hours, 13 hours, 14 hours, 23 hours, 24 hours, and the like.
In an alternative embodiment, when the mass concentration of sodium chloride is greater than the predetermined concentration, hydrogen bonds between water molecules in the aqueous solution of polyvinyl alcohol and polyvinyl alcohol are reduced, and salting-out of the aqueous solution of polyvinyl alcohol occurs, so that intermolecular aggregation of polyvinyl alcohol chains can occur, further serving as physical nodes, to form a polyvinyl alcohol network in the film.
It should be noted that, for an aqueous solution of polyvinyl alcohol (PVA), hydrogen bonds between water molecules and PVA chains dominate, so that the PVA chains are stretched in the aqueous solution and have a certain solubility. The addition of electrolytes can affect the nature and extent of hydrogen bonding in aqueous solutions of PVA. The addition of the low-concentration NaCl mainly destroys hydrogen bonds in and among PVA chain molecules, and is beneficial to the interaction of water molecules and PVA, thereby improving the solubility and viscosity of the PVA solution.
However, NaCl at a sufficiently high concentration reduces the hydrogen bonding between the water molecules and PVA, resulting in a decrease in solubility and intrinsic viscosity, accompanied by a "salting-out" effect. The film-forming liquid is dripped on the surface of the NaCl tabletting, and water molecules and NaCl form a large amount of hydrated ions, which destroy hydrogen bonds between water molecules and PVA chains, so that the PVA chains form intermolecular and intramolecular hydrogen bonds. At the same time, intermolecular aggregation of PVA chains occurs due to the "salting out" effect. The intermolecular aggregation then further acts as a physical node, creating a network of PVA chain entanglement within the film. The formation of the conforming membrane material is based on the intense competition of NaCl for water molecules, resulting in a thin film of polymer chain entangled physical network.
Therefore, the embodiment of the invention is realized by limiting the mass ratio of NaCl to the reticulating agent in the film forming solution to be not less than 10:1, the NaCl is kept at high concentration, so that intermolecular aggregation of PVA chains can occur, and finally, the composite membrane material with a three-dimensional network structure is formed.
On the other hand, the embodiment of the present application provides a soot carbon-based composite film material, please refer to fig. 2, and fig. 2 is a diagram of a composite film material SP-1 prepared by the preparation method provided in embodiment 1. The soot carbon-based composite film material is prepared by any one of the preparation methods of the soot carbon-based composite film material.
The preparation methods provided by the embodiments of the present invention will be further described below by way of alternative embodiments.
Example 1: and (3) sequentially filtering and washing the collected diesel soot carbon by using acetone and ethanol, drying for 24h in an oven at 100 ℃, and grinding. At room temperature, 0.15g of soot carbon is uniformly mixed with 3g of polyvinyl alcohol with the mass fraction of 5% and 2g of deionized water; tabletting 4g of NaCl by using a tabletting machine under the following tabletting conditions: 8.0 MPa. Dropwise adding 2.5g of mixed solution of the soot carbon and the polyvinyl alcohol onto a NaCl sheet, standing for 12h, soaking into 100mL of distilled water to remove NaCl, replacing the distilled water for three times, and freeze-drying to obtain the black soot carbon-based composite membrane SP-1. As shown in fig. 3, SP-1 has a multi-stage three-dimensional network structure.
Example 2: and (3) sequentially filtering and washing the collected diesel soot carbon by using acetone and ethanol, drying for 24h in an oven at 100 ℃, and grinding. At room temperature, 0.3g of soot carbon, 3g of polyvinyl alcohol with the mass fraction of 5% and 2g of deionized water are uniformly mixed; tabletting 4g of NaCl by using a tabletting machine under the following tabletting conditions: 8.0 MPa. Dropwise adding 2.5g of mixed solution of the soot carbon and the polyvinyl alcohol onto a NaCl sheet, standing for 12h, soaking into 100mL of distilled water to remove NaCl, replacing the distilled water for three times, and freeze-drying to obtain the black soot carbon-based composite membrane SP-2. As shown in FIG. 4, SP-2 also has a porous structure, a three-dimensional network is formed, the content of carbon particles in the soot is increased compared with SP-1, and the roughness of the wall surface of the pore channel is increased.
Example 3: and (3) sequentially filtering and washing the collected diesel soot carbon by using acetone and ethanol, drying for 24h in an oven at 100 ℃, and grinding. At room temperature, 0.45g of soot carbon is uniformly mixed with 3g of polyvinyl alcohol with the mass fraction of 5% and 2g of deionized water; tabletting 4g of NaCl by using a tabletting machine under the following tabletting conditions: 8.0 MPa. Dropwise adding 2.5g of mixed solution of the soot carbon and the polyvinyl alcohol onto a NaCl sheet, standing for 12h, soaking into 100mL of distilled water to remove NaCl, replacing the distilled water for three times, and freeze-drying to obtain the black soot carbon-based composite membrane SP-3. As shown in fig. 5, the soot carbon particles in SP-3 are fixedly connected by the polymer to form a network structure, and the content of the soot carbon particles is significantly increased.
The composite film material prepared by the method can be used as a light absorption material in solar interface evaporation. Referring to FIG. 6, FIG. 6 shows the composite film materials SP-1, SP-2 and SP-3 prepared in examples 1, 2 and 3 at 1 kW m-2The surface moisture evaporation capacity and the corresponding light-heat conversion efficiency schematic diagram under the simulated sunlight irradiation intensity. As can be seen from fig. 6, the composite film material prepared by the method provided by the embodiment of the invention is used as a light absorption material in solar interface evaporation, has high water evaporation amount and high photo-thermal conversion efficiency, and has good use value. In addition, the preparation method is simple and easy to operate, green and environment-friendly, has amplification potential, and can also be expanded to other material systems, such as inorganic clay, carbon nano tubes, carbon powder and the like.
The above examples merely represent some embodiments of the present invention, and the description thereof is more specific and detailed, but not to be construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present invention should be subject to the appended claims.
Claims (9)
1. A preparation method of a soot carbon-based composite membrane material is characterized by comprising the following steps:
step (1): preparing a film forming solution, wherein the film forming solution comprises a granular film forming substrate and a net forming agent, the net forming agent can enable the film forming substrate to form a three-dimensional network structure, the granular film forming substrate is soot carbon, and the net forming agent is a polyvinyl alcohol aqueous solution;
step (2): preparing a sodium chloride tablet, wherein the sodium chloride tablet is used for forming the composite membrane material with the three-dimensional network structure through polyvinyl alcohol in the film-forming solution when the film-forming solution is in contact with the sodium chloride tablet;
and (3): preparing a composite membrane material, dropwise adding the film forming solution on a sodium chloride pressing sheet, separating out liquid in the polyvinyl alcohol by the sodium chloride pressing sheet, and solidifying the soot carbon to form the composite membrane material with the three-dimensional network structure;
wherein the mass ratio of the sodium chloride tabletting to the polyvinyl alcohol in the film-forming solution is not less than 10: 1.
2. the method for preparing a soot carbon-based composite film material as claimed in claim 1, wherein the mass concentration of the aqueous solution of polyvinyl alcohol in the step (1) is not less than 5%.
3. The method for preparing a soot carbon-based composite film material as claimed in claim 2, wherein when the mass concentration of the sodium chloride pellet in the step (3) is greater than a predetermined concentration, hydrogen bonds between water molecules and polyvinyl alcohol in the aqueous solution of polyvinyl alcohol are reduced, and the aqueous solution of polyvinyl alcohol is salted out; the polyvinyl alcohol chains are subjected to intermolecular aggregation and further serve as physical nodes to form the three-dimensional network structure in the film.
4. The method for preparing a soot carbon-based composite film material as claimed in claim 1, wherein the step of preparing the deposition solution in step (1) comprises: and washing the soot carbon by using acetone and ethanol in sequence, drying at a preset temperature for a first preset time, and grinding to obtain the film-forming matrix.
5. The method for preparing a soot carbon-based composite film material as claimed in claim 1, wherein the mass ratio of the film-forming substrate to the polyvinyl alcohol in the film-forming solution of step (1) is 1:1 to 5.
6. The method for preparing a soot carbon-based composite film material as claimed in claim 1, wherein the mass concentration of the film-forming substrate in the film-forming solution in the step (1) is 2.9% to 10.7%.
7. The method for preparing a soot carbon-based composite membrane material as claimed in claim 1, wherein the step of dropping the deposition solution on the sodium chloride pellet in the step (3) comprises dropping the deposition solution on the sodium chloride pellet, standing for a second predetermined time, soaking in distilled water, and freeze-drying to obtain the composite membrane material.
8. The method for preparing a soot carbon-based composite film material according to claim 7, wherein the second predetermined time is 12 hours to 24 hours.
9. The method for preparing the soot carbon-based composite film material as claimed in claim 4, wherein the preset temperature is 80 ℃ to 120 ℃, and the first preset time is 12 hours to 24 hours.
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