CN111318183B - Graphene nanofiber hollow filter rod and preparation method thereof - Google Patents
Graphene nanofiber hollow filter rod and preparation method thereof Download PDFInfo
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- 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
- B01D71/48—Polyesters
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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
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- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/08—Hollow fibre membranes
Abstract
The invention discloses a graphene nanofiber hollow filter rod and a preparation method thereof, wherein the graphene nanofiber hollow filter rod comprises a supporting framework cylinder and a filter material layer coated outside the supporting framework cylinder; the filter material layer is characterized by being prepared from the following raw materials in parts by weight: 30.0 to 35.0 portions of graphene nano fiber, 8.0 to 10.0 portions of polylactic acid fiber, 0.8 to 1.3 portions of calcium carbonate, 3.2 to 3.8 portions of modified nano titanium dioxide and 2.0 to 2.5 portions of ethyl cellulose. The graphene nanofiber hollow filter rod prepared by the invention is of a hollow structure, has a large specific surface area, and has the characteristics of high-efficiency filtration, good heat resistance, stability, durability, high safety and long service life.
Description
Technical Field
The invention relates to the technical field of hollow filter rods, in particular to a graphene nanofiber hollow filter rod and a preparation method thereof.
Background
With the improvement of living standard, people put higher requirements on the quality of drinking water, and therefore, the water purifying filter is widely applied. It is understood that the filter element in the traditional water purifying filter has three kinds, the first kind is the simply mixed particle filter material, the second kind is the mixture of the extrusion forming particle filter material and the rubber powder, and the third kind is the mixture of the sintering forming particle filter material and the macromolecule rubber powder; the particle filter materials adopted in the three filter elements have small specific surface area, can not purify water efficiently, and can not utilize fiber-based materials, so that the limitation of raw materials is large.
The graphene nanofiber prepared from the nanoscale graphene oxide has the characteristics of high strength, good toughness and light weight, has excellent heat transfer conductivity, is dispersed in a material matrix, is firmer, has a larger specific surface area, can be further applied to a filter material, and enhances the filtering efficiency.
Chinese patent CN109364582A discloses a ceramic nanofiber hollow filter rod, which comprises a supporting framework cylinder and a filter material layer sleeved outside the supporting framework cylinder, wherein the filter material layer comprises the following materials in parts by weight: 50-75 parts of short-fiber aluminum fiber, 10-30 parts of nano fiber, 8-25 parts of calcium carbonate and 5-15 parts of adhesive. However, the ceramic nanofiber hollow filter rod disclosed by the invention is poor in toughness, low in mechanical strength and short in service life, and needs to be further improved.
Chinese patent CN108704384A discloses a water purifying filter rod, which comprises a first pipe body, a second pipe body and a third pipe body; the first pipe body, the second pipe body and the third pipe body are all made of antibacterial PVC plastic. The water purifying filter rod is made of antibacterial, low-temperature-resistant and sanitary materials, is simple, quick and environment-friendly, and is used for filtering tap water and removing rust, heavy metals, peculiar smell, algae, bacteria, chemical residues and the like in a water conveying pipeline and water storage equipment. However, the water purifying filter rod in the invention has poor filtering effect, the filter rod needs to be replaced frequently, and the cost is high.
Therefore, the invention provides a graphene nanofiber hollow filter rod and a preparation method thereof, the graphene nanofiber and polylactic acid fiber are combined, modified nano titanium dioxide is used as an auxiliary material, the prepared filter rod is of a hollow structure, the specific surface area is large, and the problems of low efficiency, limited raw material selection and short service life of the traditional water purification filter can be solved.
Disclosure of Invention
Aiming at the problems, the invention provides a graphene nanofiber hollow filter rod and a preparation method thereof.
The technical scheme adopted by the invention for solving the problems is as follows: a graphene nanofiber hollow filter rod comprises a supporting framework cylinder and a filter material layer coated outside the supporting framework cylinder; the filtering material layer is prepared from the following raw materials in parts by weight: 30.0 to 35.0 portions of graphene nano fiber, 8.0 to 10.0 portions of polylactic acid fiber, 0.8 to 1.3 portions of calcium carbonate, 3.2 to 3.8 portions of modified nano titanium dioxide and 2.0 to 2.5 portions of ethyl cellulose.
The graphene nanofiber has the advantages of large specific surface area, good toughness, high strength and excellent mechanical property, the polylactic acid fiber has good biocompatibility, biological absorbability and heat resistance, calcium carbonate is decomposed in the heating process to form uniform pores, the water quality can be filtered and purified, the modified nano titanium dioxide has high surface activity, the modified nano titanium dioxide is filled between the graphene nanofiber and the polylactic acid fiber to form a stable system, the heat resistance and the stability of the polylactic acid fiber are improved, the mechanical strength is improved, the ethyl cellulose is filled between the graphene nanofiber and the polylactic acid fiber, the bonding strength between the graphene nanofiber is improved, and the use of an adhesive is reduced.
Further, the filtering material layer is prepared from the following raw materials in parts by weight: 32.0 to 34.0 parts of graphene nano fiber, 8.5 to 9.5 parts of polylactic acid fiber, 0.9 to 1.2 parts of calcium carbonate, 3.3 to 3.7 parts of modified nano titanium dioxide and 2.1 to 2.4 parts of ethyl cellulose.
Further, the preparation method of the modified nano titanium dioxide comprises the following steps:
step a, dissolving hexadecyl trimethyl ammonium chloride and hexadecyl pyridine chloride in deionized water, and stirring for 10-15 minutes to obtain a solution A;
b, adding nano titanium dioxide into the solution A obtained in the step a, keeping the temperature and stirring for 60-90 minutes at 85-125 ℃, and then performing suction filtration, washing and drying to obtain a product;
roasting the product obtained in the step c and the step b for 3 to 6 hours at the temperature of 320 to 420 ℃, then preserving the heat for 2 to 4 hours at the temperature of 220 to 260 ℃, finally cooling to room temperature, and crushing to obtain the modified nano titanium dioxide.
Furthermore, in the step a, the mass ratio of the hexadecyl trimethyl ammonium chloride to the hexadecyl pyridine chloride to the deionized water is 1: 0.8-1.2: 8.
furthermore, in the step b, the ratio of the solution A to the nano titanium dioxide is 10 mL: 0.5g to 1.0 g.
Another object of the present invention is to provide a method for preparing the graphene nanofiber hollow filter rod, which comprises the following steps:
step I, shearing and dispersing the graphene nano fibers and the polylactic acid fibers in deionized water for 30-40 minutes for the first time, and then adding the calcium carbonate, the modified nano titanium dioxide and the ethyl cellulose in parts by weight for 20-30 minutes for the second time to obtain a mixture;
and step II, coating the mixture obtained in the step I outside a supporting framework cylinder by utilizing negative pressure adsorption to form a filter material layer, and then carrying out hot press forming on the filter material layer to obtain the graphene nanofiber hollow filter rod.
Further, in the step I, the first shearing and dispersing speed is 2000 to 2500 revolutions per minute, and the second shearing and dispersing speed is 1500 to 2000 revolutions per minute.
Further, in step II, the hot press forming specifically includes: firstly, heating the filter material layer to 85-115 ℃ under the condition that the pressure is 2.5-5.5 MPa, keeping the temperature for 30-90 minutes, then adjusting the pressure to 0.2-0.8 MPa, heating to 120-130 ℃ again, keeping the temperature for 10-40 minutes, stopping heating, naturally cooling to 45-65 ℃ and then releasing the pressure.
Further, in the step II, the thickness of the filter material layer is 6.0 mm-7.0 mm.
The invention has the advantages that:
(1) the graphene nanofiber hollow filter rod prepared by the invention is of a hollow structure, has a large specific surface area, and has the characteristics of high-efficiency filtration, good heat resistance, stability, durability, high safety and long service life;
(2) according to the graphene nanofiber hollow filter rod prepared by the invention, the fiber base material is selected, the selection range of the filter material is expanded, the use of an adhesive is reduced, the use safety is improved, the raw material cost is reduced, and the resources are saved;
(3) in the preparation process of the graphene nanofiber hollow filter rod, the pollution to the environment is low, the energy consumption is low, the preparation method is simple, the selected raw materials are environment-friendly, and the preparation method is suitable for popularization.
Detailed Description
The following detailed description of embodiments of the invention, but the invention can be practiced in many different ways, as defined and covered by the claims.
Example 1
Graphene nanofiber hollow filter rod
The filter material layer is coated outside the support framework cylinder; the filtering material layer is prepared from the following raw materials in parts by weight: 30.0kg of graphene nano-fibers, 8.0kg of polylactic acid fibers, 0.8kg of calcium carbonate, 3.2kg of modified nano-titanium dioxide and 2.0kg of ethyl cellulose; the preparation method of the modified nano titanium dioxide comprises the following steps:
step a, dissolving hexadecyl trimethyl ammonium chloride and hexadecyl pyridine chloride in deionized water, and stirring for 10 minutes to obtain a solution A; wherein the mass ratio of the hexadecyl trimethyl ammonium chloride to the hexadecyl pyridine chloride to the deionized water is 1: 0.8: 8;
b, adding nano titanium dioxide into the solution A obtained in the step a, keeping the temperature and stirring for 60 minutes at 85 ℃, and then performing suction filtration, washing and drying to obtain a product; wherein the ratio of the solution A to the nano titanium dioxide is 10 mL: 0.5 g;
and c, roasting the product obtained in the step b for 3 hours at the temperature of 320 ℃, then preserving the heat for 2 hours at the temperature of 220 ℃, finally cooling to room temperature, and crushing to obtain the modified nano titanium dioxide.
The preparation steps are as follows:
i, shearing and dispersing the graphene nano fibers and the polylactic acid fibers in deionized water at a speed of 2000 rpm for 30 minutes for the first time, then adding the calcium carbonate, the modified nano titanium dioxide and the ethyl cellulose in parts by weight, and shearing and dispersing at a speed of 1500 rpm for 20 minutes for the second time to obtain a mixture;
and step II, coating the mixture obtained in the step I outside a supporting framework cylinder by utilizing negative pressure adsorption to form a filtering material layer with the thickness of 6.0mm, heating the filtering material layer to 85 ℃ under the condition that the pressure is 2.5MPa, keeping the temperature for 30 minutes, adjusting the pressure to 0.2MPa, heating to 120 ℃ again, keeping the temperature for 10 minutes, stopping heating, naturally cooling to 45 ℃, and releasing the pressure to obtain the graphene nanofiber hollow filter rod.
The graphene nanofiber hollow filter rod prepared in the above embodiment is used for filtering tap water, and the TDS value of the filtered tap water is 12.8 mg/L.
Example 2
Graphene nanofiber hollow filter rod
The filter material layer is coated outside the support framework cylinder; the filtering material layer is prepared from the following raw materials in parts by weight: 35.0kg of graphene nano fibers, 10.0kg of polylactic acid fibers, 1.3kg of calcium carbonate, 3.8kg of modified nano titanium dioxide and 2.5kg of ethyl cellulose; the preparation method of the modified nano titanium dioxide comprises the following steps:
step a, dissolving hexadecyl trimethyl ammonium chloride and hexadecyl pyridine chloride in deionized water, and stirring for 15 minutes to obtain a solution A; wherein the mass ratio of the hexadecyl trimethyl ammonium chloride to the hexadecyl pyridine chloride to the deionized water is 1: 1.2: 8;
b, adding nano titanium dioxide into the solution A obtained in the step a, keeping the temperature and stirring for 90 minutes at the temperature of 125 ℃, and then performing suction filtration, washing and drying to obtain a product; wherein the ratio of the solution A to the nano titanium dioxide is 10 mL: 1.0 g;
and c, roasting the product obtained in the step b for 6 hours at the temperature of 420 ℃, then preserving the heat for 4 hours at the temperature of 260 ℃, finally cooling to room temperature, and crushing to obtain the modified nano titanium dioxide.
The preparation steps are as follows:
i, shearing and dispersing the graphene nano fibers and the polylactic acid fibers in deionized water at a speed of 2500 rpm for 40 minutes for the first time, then adding the calcium carbonate, the modified nano titanium dioxide and the ethyl cellulose in parts by weight, and shearing and dispersing the calcium carbonate, the modified nano titanium dioxide and the ethyl cellulose at a speed of 2000 rpm for 30 minutes for the second time to obtain a mixture;
and step II, coating the mixture obtained in the step I outside a supporting framework cylinder by utilizing negative pressure adsorption to form a filtering material layer with the thickness of 7.0mm, heating the filtering material layer to 115 ℃ under the condition that the pressure is 5.5MPa, keeping the temperature for 90 minutes, adjusting the pressure to 0.8MPa, heating to 130 ℃ again, stopping heating after keeping the temperature for 40 minutes, and releasing the pressure after naturally cooling to 65 ℃ to obtain the graphene nanofiber hollow filter rod.
The graphene nanofiber hollow filter rod prepared in the above embodiment is used for filtering tap water, and the TDS value of the filtered tap water is 12.6 mg/L.
Example 3
Graphene nanofiber hollow filter rod
The filter material layer is coated outside the support framework cylinder; the filtering material layer is prepared from the following raw materials in parts by weight: 32.0kg of graphene nano fibers, 8.5kg of polylactic acid fibers, 0.9kg of calcium carbonate, 3.3kg of modified nano titanium dioxide and 2.1kg of ethyl cellulose; the preparation method of the modified nano titanium dioxide comprises the following steps:
step a, dissolving hexadecyl trimethyl ammonium chloride and hexadecyl pyridine chloride in deionized water, and stirring for 11 minutes to obtain a solution A; wherein the mass ratio of the hexadecyl trimethyl ammonium chloride to the hexadecyl pyridine chloride to the deionized water is 1: 0.9: 8;
b, adding nano titanium dioxide into the solution A obtained in the step a, keeping the temperature and stirring for 70 minutes at the temperature of 95 ℃, and then performing suction filtration, washing and drying to obtain a product; wherein the ratio of the solution A to the nano titanium dioxide is 10 mL: 0.6 g;
and c, roasting the product obtained in the step b for 4 hours at the temperature of 340 ℃, then preserving the heat for 2.5 hours at the temperature of 230 ℃, finally cooling to room temperature, and crushing to obtain the modified nano titanium dioxide.
The preparation steps are as follows:
i, shearing and dispersing the graphene nano fibers and the polylactic acid fibers in deionized water at a speed of 2100 revolutions per minute for 32 minutes for the first time, then adding the calcium carbonate, the modified nano titanium dioxide and the ethyl cellulose in parts by weight, and shearing and dispersing at a speed of 1600 revolutions per minute for 22 minutes for the second time to obtain a mixture;
and step II, coating the mixture obtained in the step I outside a supporting framework cylinder by utilizing negative pressure adsorption to form a filtering material layer with the thickness of 6.2mm, heating the filtering material layer to 95 ℃ under the condition that the pressure is 3.5MPa, keeping the temperature for 40 minutes, adjusting the pressure to 0.3MPa, heating to 122 ℃ again, keeping the temperature for 20 minutes, stopping heating, naturally cooling to 50 ℃, and releasing the pressure to obtain the graphene nanofiber hollow filter rod.
The graphene nanofiber hollow filter rod prepared in the above example is used for filtering tap water, and the TDS value of the filtered tap water is 13.2 mg/L.
Example 4
Graphene nanofiber hollow filter rod
The filter material layer is coated outside the support framework cylinder; the filtering material layer is prepared from the following raw materials in parts by weight: 34.0kg of graphene nano fibers, 9.5kg of polylactic acid fibers, 1.2kg of calcium carbonate, 3.7kg of modified nano titanium dioxide and 2.4kg of ethyl cellulose; the preparation method of the modified nano titanium dioxide comprises the following steps:
step a, dissolving hexadecyl trimethyl ammonium chloride and hexadecyl pyridine chloride in deionized water, and stirring for 14 minutes to obtain a solution A; wherein the mass ratio of the hexadecyl trimethyl ammonium chloride to the hexadecyl pyridine chloride to the deionized water is 1: 1.1: 8;
b, adding nano titanium dioxide into the solution A obtained in the step a, keeping the temperature and stirring for 80 minutes at the temperature of 115 ℃, and then performing suction filtration, washing and drying to obtain a product; wherein the ratio of the solution A to the nano titanium dioxide is 10 mL: 0.9 g;
and c, roasting the product obtained in the step b for 5 hours at the temperature of 400 ℃, then preserving the heat for 3.5 hours at the temperature of 250 ℃, finally cooling to room temperature, and crushing to obtain the modified nano titanium dioxide.
The preparation steps are as follows:
i, shearing and dispersing the graphene nano fibers and the polylactic acid fibers in deionized water at the speed of 2400 revolutions per minute for 38 minutes for the first time, then adding the calcium carbonate, the modified nano titanium dioxide and the ethyl cellulose in parts by weight, and shearing and dispersing the calcium carbonate, the modified nano titanium dioxide and the ethyl cellulose at the speed of 1900 revolutions per minute for the second time for 28 minutes to obtain a mixture;
and step II, coating the mixture obtained in the step I outside a supporting framework cylinder by utilizing negative pressure adsorption to form a filtering material layer with the thickness of 6.8mm, heating the filtering material layer to 105 ℃ under the condition that the pressure is 4.5MPa, keeping the temperature for 80 minutes, adjusting the pressure to 0.6MPa, heating to 128 ℃ again, keeping the temperature for 30 minutes, stopping heating, naturally cooling to 60 ℃, and releasing the pressure to obtain the graphene nanofiber hollow filter rod.
The graphene nanofiber hollow filter rod prepared in the above embodiment is used for filtering tap water, and the TDS value of the filtered tap water is 12.8 mg/L.
Example 5
Graphene nanofiber hollow filter rod
The filter material layer is coated outside the support framework cylinder; the filtering material layer is prepared from the following raw materials in parts by weight: 33.0kg of graphene nano-fibers, 9.0kg of polylactic acid fibers, 1.0kg of calcium carbonate, 3.5kg of modified nano-titanium dioxide and 2.2kg of ethyl cellulose; the preparation method of the modified nano titanium dioxide comprises the following steps:
step a, dissolving hexadecyl trimethyl ammonium chloride and hexadecyl pyridine chloride in deionized water, and stirring for 13 minutes to obtain a solution A; wherein the mass ratio of the hexadecyl trimethyl ammonium chloride to the hexadecyl pyridine chloride to the deionized water is 1: 1: 8;
b, adding nano titanium dioxide into the solution A obtained in the step a, keeping the temperature and stirring for 75 minutes at 105 ℃, and then performing suction filtration, washing and drying to obtain a product; wherein the ratio of the solution A to the nano titanium dioxide is 10 mL: 0.8 g;
and c, roasting the product obtained in the step b for 4.5 hours at the temperature of 370 ℃, then preserving the heat for 3 hours at the temperature of 240 ℃, finally cooling to room temperature, and crushing to obtain the modified nano titanium dioxide.
The preparation steps are as follows:
step I, shearing and dispersing the graphene nano fibers and the polylactic acid fibers in deionized water at a speed of 2300 rpm for 35 minutes for the first time, then adding the calcium carbonate, the modified nano titanium dioxide and the ethyl cellulose in parts by weight, and shearing and dispersing at a speed of 1700 rpm for 25 minutes for the second time to obtain a mixture;
and step II, coating the mixture obtained in the step I outside a supporting framework cylinder by utilizing negative pressure adsorption to form a filtering material layer with the thickness of 6.5mm, heating the filtering material layer to 100 ℃ under the condition that the pressure is 4.0MPa, keeping the temperature for 60 minutes, adjusting the pressure to 0.5MPa, heating to 125 ℃ again, stopping heating after keeping for 25 minutes, and releasing the pressure after naturally cooling to 55 ℃ to obtain the graphene nanofiber hollow filter rod.
The graphene nanofiber hollow filter rod prepared in the above embodiment is used for filtering tap water, and the TDS value of the filtered tap water is 13.0 mg/L.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A graphene nanofiber hollow filter rod comprises a supporting framework cylinder and a filter material layer coated outside the supporting framework cylinder; the filter material layer is characterized by being prepared from the following raw materials in parts by weight: 30.0 to 35.0 portions of graphene nano fiber, 8.0 to 10.0 portions of polylactic acid fiber, 0.8 to 1.3 portions of calcium carbonate, 3.2 to 3.8 portions of modified nano titanium dioxide and 2.0 to 2.5 portions of ethyl cellulose;
the preparation method of the modified nano titanium dioxide comprises the following steps:
step a, dissolving hexadecyl trimethyl ammonium chloride and hexadecyl pyridine chloride in deionized water, and stirring for 10-15 minutes to obtain a solution A;
b, adding nano titanium dioxide into the solution A obtained in the step a, keeping the temperature and stirring for 60-90 minutes at 85-125 ℃, and then performing suction filtration, washing and drying to obtain a product;
roasting the product obtained in the step c and the step b for 3 to 6 hours at the temperature of 320 to 420 ℃, then preserving the heat for 2 to 4 hours at the temperature of 220 to 260 ℃, finally cooling to room temperature, and crushing to obtain the modified nano titanium dioxide.
2. The graphene nanofiber hollow filter rod according to claim 1, wherein the filter material layer is prepared from the following raw materials in parts by weight: 32.0 to 34.0 parts of graphene nano fiber, 8.5 to 9.5 parts of polylactic acid fiber, 0.9 to 1.2 parts of calcium carbonate, 3.3 to 3.7 parts of modified nano titanium dioxide and 2.1 to 2.4 parts of ethyl cellulose.
3. The graphene nanofiber hollow filter rod according to claim 1, wherein in the step a, the mass ratio of the cetyltrimethylammonium chloride to the cetylpyridinium chloride to the deionized water is 1: 0.8-1.2: 8.
4. the graphene nanofiber hollow filter rod according to claim 1, wherein in the step b, the ratio of the solution A to the nano titanium dioxide is 10 mL: 0.5g to 1.0 g.
5. A preparation method of the graphene nanofiber hollow filter rod as claimed in any one of claims 1 to 4, characterized by comprising the following steps:
step I, shearing and dispersing the graphene nano fibers and the polylactic acid fibers in deionized water for 30-40 minutes for the first time, and then adding the calcium carbonate, the modified nano titanium dioxide and the ethyl cellulose in parts by weight for 20-30 minutes for the second time to obtain a mixture;
and step II, coating the mixture obtained in the step I outside a supporting framework cylinder by utilizing negative pressure adsorption to form a filter material layer, and then carrying out hot press forming on the filter material layer to obtain the graphene nanofiber hollow filter rod.
6. The method of claim 5, wherein in step I, the first shear dispersion rate is from 2000 to 2500 rpm, and the second shear dispersion rate is from 1500 to 2000 rpm.
7. The preparation method according to claim 5, wherein in step II, the hot press forming is specifically: firstly, heating the filter material layer to 85-115 ℃ under the condition that the pressure is 2.5-5.5 MPa, keeping the temperature for 30-90 minutes, then adjusting the pressure to 0.2-0.8 MPa, heating to 120-130 ℃ again, keeping the temperature for 10-40 minutes, stopping heating, naturally cooling to 45-65 ℃ and then releasing the pressure.
8. The method according to claim 5, wherein in step II, the thickness of the filter material layer is 6.0mm to 7.0 mm.
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