CN109569097B - Graphene sandwich composite PP cotton filter element and preparation method thereof - Google Patents
Graphene sandwich composite PP cotton filter element and preparation method thereof Download PDFInfo
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- CN109569097B CN109569097B CN201811505646.XA CN201811505646A CN109569097B CN 109569097 B CN109569097 B CN 109569097B CN 201811505646 A CN201811505646 A CN 201811505646A CN 109569097 B CN109569097 B CN 109569097B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/14—Other self-supporting filtering material ; Other filtering material
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
Abstract
The invention mainly provides a graphene sandwich composite PP cotton filter element and a preparation method thereof, wherein the filter element comprises a polypropylene layer and a graphene composite polypropylene layer, and the graphene composite polypropylene layer is arranged on the outer side of a common polypropylene layer; the graphene composite polypropylene layer comprises the following components in percentage by mass: 96-99.6% of polypropylene; 0.1-2.0% of modified graphene oxide; 0.1 to 1.0 percent of binder; 0.1 to 1.0 percent of antioxidant; 0.1 to 0.5 percent of cooling auxiliary agent. And the double melt-blown machines adopted in the preparation process perform melt-blown spinning successively, and the graphene composite PP layer is rapidly melt-blown after the first common PP layer, so that the two layers are tightly combined. The obtained filter element has excellent filtering effect and antibacterial property.
Description
Technical Field
The invention belongs to the technical field of sewage purification filter elements, and particularly relates to a graphene sandwich composite PP cotton filter element and a preparation method thereof.
Background
Polypropylene (PP) is a semi-crystalline thermoplastic. Has high impact resistance, high mechanical property and high resistance to corrosion of various organic solvents and acid and alkali. Has wide application in industry, and is one of the common polymer materials.
The meltblown process is one type of polymer extrusion nonwoven process. From the 20 th century and the 50 th century, companies in the united states began researching the production of polystyrene ultrafine fiber nonwoven fabrics by the air jet-electrospinning method, and the process gradually occupied a certain market scale through the sixty-seventies. The melt-spraying type pp filter element is a tubular filter element which is mainly made of nontoxic and tasteless polyester fiber particles through heating, melting, spinning, drawing and receiving forming; if the raw material is mainly polyester fiber, the filter element can be called a PP melt-blown filter element.
The fibers of the polypropylene filter element randomly form a three-dimensional microporous structure in space, the pore diameters of pores are distributed in a gradient manner along the flow direction of filtrate, and the surface, deep layer and fine filtration are integrated, so that impurities with different particle sizes can be intercepted. The precision range of the filter element is 0.5-100 mu m. Can be generally used as the pre-filtration of a water purifier, the primary filtration of sewage treatment and the like.
The filter element of the water purifier generally comprises a polypropylene filter element, an active carbon filter element, a resin filter element, a ro membrane filter element and the like. The sewage treatment process mainly has three stages, wherein the first-stage sewage treatment is also called as sewage physical treatment. Through simple precipitation, filtration or proper aeration, suspended matters in the sewage are removed, the pH value is adjusted, and the rotting degree of the sewage is reduced. The treatment can be composed of screening, gravity precipitation, flotation and other methods which are connected in series, and most of particulate matters with the particle size of more than 100 microns in the sewage are removed. Larger substances can be removed by screening; gravity precipitation removes inorganic particles and organic particles with a relative density greater than 1 that are agglomerated.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a graphene sandwich composite PP cotton filter element and a preparation method thereof. The invention comprises a preparation formula of melt-blown masterbatch and a layer of graphene composite PP cotton melt-blown on the outer side of a common PP filter element in the same ratio, and aims to enhance the filtering effect and the antibacterial property of the filter element. And (3) opening the common melt-blowing machine, spraying a layer of common polypropylene layer on the screw, opening the graphene composite master batch melt-blowing machine after 3-5 seconds, and rapidly melt-blowing the graphene composite pp layer after the first layer of common pp layer to enable the two layers to be tightly combined.
The purpose of the invention is realized by the following technical scheme:
the invention provides a graphene sandwich composite PP cotton filter element which comprises a common polypropylene layer and a graphene composite polypropylene layer, wherein the graphene composite polypropylene layer is arranged on the outer side of the polypropylene layer;
the graphene composite polypropylene layer comprises the following components in percentage by mass:
preferably, the content of the modified graphene oxide is 1-2%.
Preferably, the preparation method of the modified graphene oxide comprises the following steps:
a1, carrying out ultrasonic dispersion on graphene oxide to obtain a graphene dispersion solution, then adding an organic modified monomer, heating to 50-95 ℃, and carrying out high-speed stirring reaction to obtain grafted modified graphene oxide;
and A2, drying the grafted modified graphene oxide, and performing jet milling and sieving to obtain the modified graphene oxide.
Preferably, the organic modified monomer is at least one of polyurethane modified monomer and acrylate modified monomer; the addition amount of the organic modified monomer is 0.1-2% of the mass of the graphene oxide.
Preferably, the thickness of the graphene composite polypropylene layer is 1-5mm, more preferably 3-5 mm.
Preferably, the binder is selected from at least one of synthetic resin, rubber particles; the antioxidant is selected from at least one of BHA and Propyl Gallate (PG); the cooling auxiliary agent is at least one of PP cooling master batch and PE cooling master batch.
The invention also provides a preparation method of the graphene sandwich composite PP cotton filter element, which comprises the following steps:
s1, uniformly mixing polypropylene and modified graphene oxide according to a proportion, simultaneously mixing an antioxidant, a nucleating agent and a cooling aid, and extruding, drawing, air-drying the surface of the prepared mixture, and granulating to obtain graphene-polypropylene composite master batches;
s2, melt-blowing polypropylene slices on a spinning roller to form a polypropylene layer, then quickly melt-blowing graphene-polypropylene composite master batches on the polypropylene layer to form a graphene composite polypropylene layer, shaping and cutting to obtain the graphene sandwich composite PP cotton filter core.
Preferably, in the step S1, the extrusion temperature is 200-280 ℃.
Preferably, in step S2, the polypropylene chips have a melt-blowing temperature of 180 to 280 ℃ and a spinning speed of 1.5 × 10-7L/min～2×10-7L/min。
Preferably, in step S2, the graphene-polypropylene composite masterbatch is melt-blown at a temperature of 220 to 360 ℃ and at a spinning speed of 0.8 × 10-7L/min～1.2×10-7L/min。
The melt-blowing temperature of the polypropylene white chips and the graphene composite master batches is calculated according to the specific melt index, the temperature is too high, the melt-blowing is easy to liquefy, and the melt-blowing is solidified into a plastic body after being sprayed, so that the water is not easy to pass through; if the temperature is too low, the melting temperature of the particles is not reached, and the spinning cannot be performed.
Preferably, in the step S2, the shaping is performed by hot air, and the air blowing temperature is 80-120 ℃.
After the filter element is formed and at a distance before cutting, a hot air blower is arranged to blow the surface of the filter element, and mainly the temperature balance of the surface of the filter element is kept, so that the spinning on the surface is further and tightly combined. If the temperature of the jet air is too high, the surface can be melted into liquid, so that a channel for spinning is blocked, and water is not favorably fed; on the contrary, if the temperature is too low, the spinning on the surface of the filter element can generate concave-convex spinning, and fine spinning easily enters water in the filtering process to cause certain harm.
Compared with the prior art, the invention has the following beneficial effects:
1. the outer layer of the filter element is formed by compounding graphene and pp, so that the filter element has an obvious antibacterial effect, and embodies the healthy, safe and green concept;
2. the special bacteriostatic function of the graphene composite pp cotton filter element is not easy to be blocked by bacteria and impurities, so that the water flux is larger, and the filtered water amount is larger;
3. the service life of the filter element is longer than that of the common filter element, and on the premise of ensuring the filtering effect, the outer wall of the common pp filter element is easily blocked by impurities such as bacteria and the like, so that water cannot pass through the common pp filter element, and the utilization rate of the inside of the pp filter element is low. And the surface of the sandwich type composite PP cotton filter element is antibacterial and is not easy to block. The integral filtering performance can be better utilized;
4. the composite pp filter element is a preliminary filtering model, the hierarchical filtering from top to bottom is an innovation, and other filtering materials such as a layer of detergent and the like can be compounded between the inner side and the outer side of the ordinary pp layer and the graphene composite pp layer, so that the descaling performance of the filter element is improved.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that it would be obvious to those skilled in the art that various changes and modifications can be made without departing from the spirit of the invention. All falling within the scope of the present invention.
In the following examples, the organic modifying monomer used is at least one of a polyurethane modifying monomer and an acrylate modifying monomer; the addition amount of the organic modified monomer is 0.1-2% of the mass of the graphene oxide.
The adopted binder is selected from at least one of synthetic resin and rubber particles; the antioxidant is selected from at least one of BHA and Propyl Gallate (PG); the cooling auxiliary agent is at least one of PP cooling master batch and PE cooling master batch.
Example 1
The embodiment provides a graphene sandwich composite PP cotton filter element, which comprises a polypropylene layer and a graphene composite polypropylene layer, wherein the graphene composite polypropylene layer is arranged on the outer side of a common polypropylene layer;
the preparation method of the graphene sandwich composite PP cotton filter element comprises the following steps:
1. preparing graphene oxide by adopting an improved Hummers method, and then uniformly dispersing the graphene oxide into an aqueous solution under the action of ultrasonic waves;
2. adding an organic modified monomer (1% of a polyurethane modified monomer) into the graphene dispersion liquid prepared in the step (1), raising the temperature to 50-95 ℃, stirring at a high speed for reaction to prepare grafted modified graphene oxide, filtering the modified graphene oxide to remove moisture, drying in vacuum, and carrying out airflow crushing and sieving to obtain modified graphene oxide powder;
3. uniformly mixing the graphene powder prepared in the step 2 with polypropylene powder according to the proportion shown in the table 1, simultaneously mixing 0.1% of antioxidant, 0.1% of nucleating agent and 0.1% of cooling aid powder, and extruding, drafting, surface air-drying and dicing the prepared mixture at 200-280 ℃ by using an extruder to obtain graphene-polypropylene composite master batches;
4. the composite master batch is placed in a melt spinning machine 2, common polypropylene slices are placed in a melt spinning machine 1, and the air volume is adjusted for melt spinning.
5. In the melt-blowing process, the melt-blowing spinning machine 1 firstly melts and blows on the spinning roller for 3-5 seconds and then melts and blows through the melt-spinning machine 2, and then the common white polypropylene layer on the inner side and the graphene composite polypropylene layer on the outer side are obtained.
6. In the melt-blowing process, the melt-blowing temperature of the melt-spinning machine 1 is 180-280 ℃, and the spinning speed is 1.5 multiplied by 10- 7L/min-2×10-7L/min, the melt-blowing temperature of the melt-spinning machine 2 is 220-360 ℃, and the spinning speed is 0.8 multiplied by 10-7L/min-1.2×10-7L/min。
7. In the melt-blowing process, a hot air blower is required to be used for blow-molding before the filter element is molded, and the blowing temperature is 80-120 ℃.
8. And after the filter element is melt-blown and shaped, cutting the filter element by an automatic cutting machine to obtain the graphene sandwich composite filter element with the inner diameter of 30mm, the thickness of the polypropylene layer of 12mm and the thickness of the graphene composite polypropylene layer of 3 mm.
The bacteriostasis rate and water flux of the obtained graphene sandwich composite filter element are shown in table 1.
TABLE 1
Example 2
The embodiment provides a graphene sandwich composite PP cotton filter element, which comprises a polypropylene layer and a graphene composite polypropylene layer, wherein the graphene composite polypropylene layer is arranged on the outer side of the polypropylene layer;
the preparation method of the graphene sandwich composite PP cotton filter element is basically the same as that in the embodiment 1, and the prepared graphene sandwich composite filter element is 30mm in inner diameter, 15mm in total thickness of the filter element layer, 1% in the addition amount of graphene in the graphene composite polypropylene layer and shown in the table 2 in thickness of the graphene composite polypropylene layer.
The bacteriostasis rate and water flux of the obtained graphene sandwich composite filter element are shown in table 2.
TABLE 2
Example 3
The embodiment provides a graphene sandwich composite PP cotton filter element, which comprises a polypropylene layer and a graphene composite polypropylene layer, wherein the graphene composite polypropylene layer is arranged on the outer side of the polypropylene layer;
the preparation method of the graphene sandwich composite PP cotton filter element is basically the same as that in the embodiment 1, the prepared graphene sandwich composite filter element is 30mm in inner diameter, 15mm in thickness of a common filter element layer, 1% of graphene in the graphene composite polypropylene layer and the thickness of the graphene composite polypropylene layer shown in the table 3, and the total thickness of the filter element is increased along with the thickness of the graphene layer.
TABLE 3
Example 4
The embodiment provides a graphene sandwich composite PP cotton filter element, which comprises a polypropylene layer and a graphene composite polypropylene layer, wherein the graphene composite polypropylene layer is arranged on the outer side of the polypropylene layer;
the preparation method of the graphene sandwich composite PP cotton filter element is basically the same as that in the embodiment 1, the prepared graphene sandwich composite filter element is 30mm in inner diameter, 15mm in thickness of a common filter element layer, the total thickness of the filter element is increased along with the thickness of a graphene layer, the addition amount of graphene in the graphene composite polypropylene layer is 2%, and the thickness of the graphene composite polypropylene layer is shown in Table 4.
TABLE 4
Example 5
The embodiment provides a graphene sandwich composite PP cotton filter element, which comprises a polypropylene layer and a graphene composite polypropylene layer, wherein the graphene composite polypropylene layer is arranged on the outer side of the polypropylene layer;
the preparation method of the graphene sandwich composite PP cotton filter element comprises the following steps:
1. preparing graphene oxide by adopting an improved Hummers method, and then uniformly dispersing the graphene oxide into an aqueous solution under the action of ultrasonic waves;
2. adding an organic modified monomer (2% of acrylate modified monomer) into the graphene dispersion liquid prepared in the step 1, raising the temperature to 50-95 ℃, stirring at a high speed for reaction to obtain grafted modified graphene oxide, filtering the modified graphene oxide to remove water, drying in vacuum, and carrying out airflow crushing and sieving to obtain modified graphene oxide powder;
3. uniformly mixing the graphene powder prepared in the step 2 with polypropylene powder according to the proportion shown in the table 5, simultaneously mixing antioxidant, nucleating agent and cooling aid powder with the content shown in the table 5, and extruding, drafting, surface air-drying and granulating the prepared mixture at 200-280 ℃ by using an extruder to obtain graphene-polypropylene composite master batches;
4. the composite master batch is placed in a melt spinning machine 2, common polypropylene slices are placed in a melt spinning machine 1, and the air volume is adjusted for melt spinning.
5. In the melt-blowing process, the melt-blowing spinning machine 1 firstly melts and blows on the spinning roller for 3-5 seconds and then melts and blows through the melt-spinning machine 2, and then the common white polypropylene layer on the inner side and the graphene composite polypropylene layer on the outer side are obtained.
6. In the melt-blowing process, the melt-blowing temperature of the melt-spinning machine 1 is 180-280 ℃, and the spinning speed is 1.5 multiplied by 10- 7L/min-2×10-7L/min, the melt-blowing temperature of the melt-spinning machine 2 is 220-360 ℃, and the spinning speed is 0.8 multiplied by 10-7L/min-1.2×10-7L/min
7. In the melt-blowing process, a hot air blower is required to be used for blow-molding before the filter element is molded, and the blowing temperature is 80-120 ℃.
8. And after the filter element is melt-blown and shaped, cutting the filter element by an automatic cutting machine to obtain the graphene sandwich composite filter element with the inner diameter of 30mm, the thickness of the polypropylene layer of 12mm and the thickness of the graphene composite polypropylene layer of 3 mm.
TABLE 5
Comparative example 1
The comparative example provides a preparation process and a flow of a polypropylene filter element, and is different from the embodiment 1 in that common polypropylene white chips are added into two melt blowing machines for spinning. Namely, the two layers of the filter element are made of the same material. Adjusting the spinning speed and the rotating speed of the screw rod to manufacture filter elements with different thicknesses, and after the filter elements are melt-blown and shaped, cutting the filter elements by an automatic cutting machine to obtain the polypropylene filter elements with the inner diameter of 30mm and the thickness of 15 mm-20 mm. The bacteriostatic rate and water flux of the obtained filter element are shown in table 6.
TABLE 6
Comparative example 2
The comparative example provides a preparation process and a flow of a polypropylene filter element, and is different from the embodiment 1 in that graphene composite polypropylene master batches are added into two melt blowing machines for spinning. Namely, the two layers of the filter element are made of the same material. Adjusting the spinning speed and the rotating speed of the screw rod to manufacture filter elements with different thicknesses, and after the filter elements are melt-blown and shaped, cutting the filter elements by an automatic cutting machine to obtain the graphene composite polypropylene filter element with the inner diameter of 30mm and the thickness of 15 mm-20 mm. The bacteriostatic rate and water flux of the obtained filter element are shown in table 7.
TABLE 7
Comparative example 3
The comparative example provides a graphene sandwich composite PP cotton filter element, which comprises a polypropylene layer and a graphene composite polypropylene layer, wherein the graphene composite polypropylene layer is arranged on the outer side of a common polypropylene layer;
the preparation method of the graphene sandwich composite PP cotton filter element is basically the same as that of the embodiment 1, and the difference is only that: in step 2, in the comparative example, silane is used to replace a polyurethane modified monomer to modify graphene oxide.
Comparative example 4
The comparative example provides a graphene sandwich composite PP cotton filter element, which comprises a polypropylene layer and a graphene composite polypropylene layer, wherein the graphene composite polypropylene layer is arranged on the outer side of a common polypropylene layer;
the preparation method of the graphene sandwich composite PP cotton filter element is basically the same as that of the embodiment 1, and the difference is only that: in the comparative example, the graphene oxide was not modified, and the graphene oxide prepared in step 1 was directly used in step 3.
The bacteriostatic rate and water flux of the graphene sandwich composite filter elements prepared in comparative examples 3 and 4 are shown in table 8.
TABLE 8
While specific embodiments of the invention have been described above. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes or modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention. The embodiments and features of the embodiments of the present application may be combined with each other arbitrarily without conflict.
Claims (8)
1. The graphene sandwich composite PP cotton filter element is characterized by comprising a polypropylene layer and a graphene composite polypropylene layer, wherein the graphene composite polypropylene layer is arranged on the outer side of a common polypropylene layer;
the graphene composite polypropylene layer comprises the following components in percentage by mass:
the preparation method of the modified graphene oxide comprises the following steps:
a1, carrying out ultrasonic dispersion on graphene oxide to obtain a graphene dispersion solution, then adding an organic modified monomer, heating to 50-95 ℃, and carrying out high-speed stirring reaction to obtain grafted modified graphene oxide;
a2, drying the grafted modified graphene oxide, and performing jet milling and sieving to obtain the modified graphene oxide;
the organic modified monomer is at least one of modified polyurethane and modified acrylate; the addition amount of the organic modified monomer is 0.1-2% of the mass of the graphene oxide.
2. The graphene sandwich composite PP cotton filter element according to claim 1, wherein the thickness of the graphene composite polypropylene layer is 1-5 mm.
3. The graphene sandwich composite PP cotton filter element according to claim 1, wherein the binder is selected from at least one of synthetic resin and rubber particles; the antioxidant is selected from at least one of BHA and propyl gallate; the cooling auxiliary agent is at least one of PP cooling master batch and PE cooling master batch.
4. The preparation method of the graphene sandwich composite PP cotton filter element according to claim 1, characterized by comprising the following steps:
s1, uniformly mixing polypropylene and modified graphene oxide according to a proportion, simultaneously mixing an antioxidant, a nucleating agent and a cooling aid, and extruding, drawing, air-drying the surface of the prepared mixture, and granulating to obtain graphene-polypropylene composite master batches;
s2, melt-blowing polypropylene slices on a spinning roller to form a polypropylene layer, then quickly melt-blowing graphene-polypropylene composite master batches on the polypropylene layer to form a graphene composite polypropylene layer, shaping and cutting to obtain the graphene sandwich composite PP cotton filter core.
5. The preparation method of the graphene sandwich composite PP cotton filter element according to claim 4, wherein in the step S1, the extrusion temperature is 200-280 ℃.
6. The preparation method of the graphene sandwich composite PP cotton filter element according to claim 4, wherein in the step S2, the melt-blowing temperature of the polypropylene slices is 180-280 ℃, and the spinning speed is 1.5 x 10-7L/min～2×10-7L/min。
7. The preparation method of the graphene sandwich composite PP cotton filter element according to claim 4, wherein in the step S2, the melt-blowing temperature of the graphene-polypropylene composite master batch is 220-360 ℃, and the spinning speed is 0.8 x 10-7L/min～1.2×10-7L/min。
8. The preparation method of the graphene sandwich composite PP cotton filter element according to claim 4, wherein in the step S2, hot air is adopted for shaping, and the air blowing temperature is 80-120 ℃.
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