• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    The present disclosure generally relates to the field of polymer materials, and, in particular, to a heterojunction composite and a process for making the same, and to an antibacterial and antistatic polymer material and a process for making the same as well as use thereof. A MWCNTs/Ag heterojunction composite comprises carbon nanotubes and nano silver particles deposited on surfaces of the carbon nanotubes. The nano silver particles are deposited on surfaces of the carbon nanotubes and have an improved dispersibility, avoiding aggregation of the nano silver particles and allowing the nano silver particles to exert their antibacterial activity effectively. The composite combines antibacterial activity of nano silver with conductivity of carbon nanotubes and has a high antibacterial activity and an excellent antistatic property.
    公开号:NL2028522A
    申请号:NL2028522
    申请日:2021-06-23
    公开日:2021-09-01
    发明作者:Luo Faliang；Ma Dequan
    申请人:Univ Ningxia；
    IPC主号:
    专利说明:

    [01] [01] This patent application claims the benefit and priority of Chinese Patent Application No. 202110468315.9 filed on April 28, 2021, the disclosure of which is incorporated by reference herein in its entirety as part of the present application.TECHNICAL FIELD
    [02] [02] The present disclosure generally relates to the field of polymer materials, and, in particular, to a heterojunction composite and a process for making the same, and to an antibacterial and antistatic polymer material and a process for making the same as well as use thereof.BACKGROUND ART
    [03] [03] Polymers have been widely used in various fields including industrial and medical fields due to their low price, easy molding workability, and excellent comprehensive properties. However, most polymer materials are insulating and have very high surface resistivity and volume resistivity. Due to these, electrostatic charges such as resulting from collisions, friction, and electrostatic induction tend to build-up on surfaces of the materials and are unlikely to disappear. Hence, the use of such polymer materials in applications requiring static free environments is limited. Moreover, these polymer materials cannot exert an effective antibacterial action, causing microbial growth thereon and thus potential hazards. This leads to inconvenience for the users, and limits their use in fields including the medical field.
    [04] [04] The current antistatic and antibacterial polymer materials available on the market are typically polymers complexed with nano silver particles which have conductivity and antibacterial effect. However, the nano silver particles present in these polymers may have low dispersibility and stability, which may adversely influence functionality of the polymer materials and lead to low antistatic and antibacterial capabilities thereof.SUMMARY
    [05] [05] In view of the above problems, the present disclosure provides a heterojunction composite and a process for making the same. Further, the present disclosure provides an antibacterial and antistatic polymer material and a process for making the same as well as use thereof. The heterojunction composite combines a high antibacterial activity of nano silver with a high conductivity of carbon nano tubes (CNTs), and overcomes the problem with the prior art polymer materials that the nano silver particles have low dispersibility and tend to agglomerate, as described above.
    [06] [06] Accordingly, one objective of the present disclosure is to provide a MWCNTs/Ag heterojunction composite comprising carbon nanotubes and nano silver particles deposited on surfaces of the carbon nanotubes.
    [07] [07] Preferably, the nano silver particles have a particle size of 3 to 15 nanometers (nm).
    [08] [08] Preferably, a mass ratio of the nano silver particles to the CNTs is within a range of 0.19 to 0.23.
    [09] [09] Another objective of the present disclosure is to provide a process for making the MWCNTs/Ag heterojunction composite as described above, comprising steps of: mixing a soluble silver salt, carbon nanotubes, and an aqueous solution of polyethylene glycol to form a suspension; and subjecting the suspension to ultraviolet irradiation to conduct a reduction reaction so as to produce the MWCNTs/Ag heterojunction composite.
    [10] [10] Preferably, the soluble silver salt is silver nitrate.
    [11] [11] Preferably, a mass ratio of the soluble silver salt to the carbon nanotubes is within a range of (0.5-5):(1-20).
    [12] [12] Preferably, the aqueous solution of polyethylene glycol has a molar concentration of 0.04 to 0.08 mol/L, and a ratio of mass of the soluble silver salt to volume of the aqueous solution of polyethylene glycol is within a range of (0.5-5) g:(50- 500)ml.
    [13] [13] Preferably, the ultraviolet radiation is emitted from an ultraviolet radiation source with a wavelength of 100 to 365 nm and power of 15 to 25 watts (W).
    [14] [14] Preferably, the reduction reaction is conducted at a temperature of 30 to 80 °C for 4 to 8 hours.
    [15] [15] Yet another objective of the present disclosure is to provide an antibacterial and antistatic polymer material comprising a polymer and the MWCNTs/Ag heterojunction composite as described above or the MWCNTs/Ag heterojunction composite made by the process as described above.
    [16] [16] Preferably, the polymer includes polypropylene (PP), polyethylene (PE), and polylactic acid (PLA), and is 97 to 99 % by mass with respect to the total mass of the antibacterial and antistatic polymer material.
    [17] [17] A further objective of the present disclosure is to provide a process for making the antibacterial and antistatic polymer material as described above, comprising steps of: subjecting the polymer and the MWCNTs/Ag heterojunction composite to be melt blended so as to form a melt blend thereof; and subjecting the melt blend to be molded and cooled so as to produce the antibacterial and antistatic polymer material.
    [18] [18] The present disclosure provides a MWCNTs/Ag heterojunction composite, which comprises carbon nanotubes and nano silver particles deposited on surfaces of the carbon nanotubes. The nano silver particles present in the composite are deposited on surfaces of the CNTs and have an improved dispersibility. Hence, the nano silver particles can exert their antibacterial activity effectively. The composite of the present disclosure combines antibacterial activity of nano silver with conductivity of CNTs and has a high antibacterial activity and an excellent antistatic property.
    [19] [19] The present disclosure further provides an antibacterial and antistatic polymer material, which comprises a polymer and the MW CNTs/Ag heterojunction composite as described above or the MWCNTs/Ag heterojunction composite made by the process as described above. The MWCNTs/Ag heterojunction composite is uniformly dispersed in the polymer matrix. The polymer material has a high antibacterial activity and an excellent antistatic property.BRIEFT DESCRIPTION OF THE DRAWINGS
    [20] [20] FIG. 1 is a transmission electron micrograph (TEM) of a MWCNTs/Ag heterojunction composite prepared in Example 1.DETAILED DESCRIPTION OF THE EMBODIMENTS
    [21] [21] A first aspect of the present disclosure provides a MWCNTs/Ag heterojunction composite comprising carbon nanotubes and nano silver particles deposited on surfaces of the carbon nanotubes.
    [22] [22] The carbon nanotubes may be single-walled carbon nanotubes or multi-walled carbon nanotubes. In some embodiments, multi-walled carbon nanotubes may be preferred. The carbon nanotubes may have an outer diameter of 5 to 15 nm, preferably 9 to 13 nm, and a length of 10 to 50 microns (um), preferably 30 to 40 um.
    [23] [23] The nano silver particles may have a particle size of 3 to 15 nm, preferably 3 to 6 nm.
    [24] [24] A mass ratio of the nano silver particles to the carbon nanotubes may be within arange of 0.19 to 0.23, preferably 0.2 to 0.21.
    [25] [25] A second aspect of the present disclosure provides a process for making the MWCNTs/Ag heterojunction composite according to the first aspect of the disclosure, comprising steps of: mixing a soluble silver salt, carbon nanotubes, and an aqueous solution of polyethylene glycol to form a suspension; and subjecting the suspension to ultraviolet irradiation to conduct a reduction reaction so as to produce the MWCNTSs/Ag heterojunction composite.
    [26] [26] According to this process, a soluble silver salt, carbon nanotubes, and an aqueous solution of polyethylene glycol are mixed together to form a suspension. The soluble silver salt may be silver nitrate, for example. The number average molecular weight of the polyethylene glycol may be within a range of 4,000 to 8,000, preferably 4,000 to 6,000. The aqueous solution of polyethylene glycol may have a molar concentration of 0.04 to 0.08 mol/L, preferably 0.04 to 0.06 mol/L, and a ratio of mass of the soluble silver salt to volume of the aqueous solution of polyethylene glycol may be within a range of (0.5-5)g:(50-500)ml, preferably (1-3)g:(100-200)ml.
    [27] [27] A mass ratio of the soluble silver salt to the carbon nanotubes may be within a range of (0.5-5):(1-20), preferably(1-2):(3-10).
    [28] [28] The mixing step may comprise: dissolving the soluble silver salt in the aqueous solution of polyethylene glycol to form a silver salt solution; and mixing the silver salt solution with the carbon nanotubes so as to form the suspension.
    [29] [29] In this mixing step, the soluble silver salt is firstly dissolved in the aqueous solution of polyethylene glycol to form a silver salt solution. The soluble silver salt may be dissolved in the aqueous solution of polyethylene glycol with stirring at a speed of 50 to 200 rpm, preferably 100 to 200 rpm, for S to 45 minutes, preferably 15 to 30 minutes.
    [30] [30] The addition of the polyethylene glycol enables a uniform dispersion of the silver ions present in the suspension onto surfaces of the carbon nanotubes. This can facilitate uniformly depositing metallic silver resulting from reduction of silver ions onto 5 surfaces of the carbon nanotubes.
    [31] [31] According to the mixing step, after the silver salt solution is obtained, it is mixed with the carbon nanotubes so as to form the suspension. In some embodiments, the silver salt solution may be mixed with the carbon nanotubes with stirring at a speed of 50 to 200 rpm, preferably 100 to 200 rpm, for 0.5 to 2 hours, preferably 1 hour. The mixing of the silver salt solution with the carbon nanotubes is preferably carried out in the dark so as to avoid decomposition of silver nitrate caused by irradiation with light. No particular limitation is imposed on how to achieve the dark environment.
    [32] [32] After the suspension is formed, it is subjected to ultraviolet irradiation to conduct a reduction reaction so as to obtain the MWCNTs/Ag heterojunction composite.
    [33] [33] Due to the ultraviolet radiation, the polyethylene glycol in the suspension is converted to an aldehyde, which serves as a reducing agent in the reduction reaction to reduce the silver ions in the suspension to metallic silver.
    [34] [34] The process according to the second aspect of the present disclosure further comprises: after the completion of the reduction reaction, the resulting product is subjected to filtration and then drying to obtain the composite. The product may be filtered with suction. During the suction filtration, washing is preferably carried out using water and then ethanol. The water washing may be carried out 3 to 9 times, preferably 3 to 6 times. The ethanol washing may be carried out 3 to 9 times, preferably 3 to 6 times. The drying may be carried out at a temperature of 50 to 80 °C, preferably 60 to 70 °C, for 10 to 12 hours, preferably 11 to 11.5 hours.
    [35] [35] A third aspect of the present disclosure provides an antibacterial and antistatic polymer material, which comprises a polymer and the MWCNTs/Ag heterojunction composite according to the first aspect of the present disclosure or the MWCNTs/Ag heterojunction composite made by the process according to the second aspect of the present disclosure.
    [36] [36] The polymer may be polypropylene (PP), polyethylene (PE), or polylactic acid (PLA). The polymer is preferably PP. The polymer may be 97 to 99 % by mass, preferably 97.5 to 98.5 % by mass, more preferably 98 % by mass, with respect to the total mass of the antibacterial and antistatic polymer material.
    [37] [37] A fourth aspect of the present disclosure provides a process for making the antibacterial and antistatic polymer material according to the third aspect of the disclosure, comprising steps of: subjecting the polymer and the MWCNTs/Ag heterojunction composite to be melt blended so as to form a melt blend thereof; and subjecting the melt blend to be molded and cooled so as to produce the antibacterial and antistatic polymer material.
    [38] [38] According to this process, the polymer and the MWCNTs/Ag heterojunction composite are firstly melt blended to form a melt blend thereof. Preferably, the process further comprises before the blending step, subjecting the polymer and the MWCNTs/Ag heterojunction composite to be dried separately, and dripping liquid paraffin onto a surface of the dried polymer.
    [39] [39] The polymer and the MWCNTs/Ag heterojunction composite may be separately dried in an oven. The polymer may be dried in an oven at a temperature of 60 to 100 °C, preferably 60 to 80 °C, for 6 to 12 hours, preferably 6 to 8 hours. The composite may be dried in an oven at a temperature of 80 to 120 °C, preferably 90 to 100 °C, for 6 to 10 hours, preferably 6 to 8 hours.
    [40] [40] After the polymer and the composite are dried, liquid paraffin may be dripped onto a surface of the dried polymer, which is then physically mixed with the dried composite. A mass ratio of the dried polymer to the paraffin may be within a range of (800-1,000):20, preferably (900-1,000):20. The paraffin may be dripped onto a surface of the dried polymer at any rate, and the dripping rate is not particularly limited herein.
    [41] [41] The dried polymer and composite may be physically mixed with stirring at a stirring speed of 40 to 120 rpm, preferably 60 to 80 rpm, for 3 to 10 minutes, preferably 5 to 6 minutes.
    [42] [42] The polymer and composite may be melt blended in any known manner. In an embodiment, the blending may be carried out using a two-roll mill at 165 °C with its front and rear rollers having a rotation speed ratio of 1:1.35 and the front roller having a rotation speed of 10 to 20 rpm. The blending is preferably carried out for 8 to 20 minutes, more preferably 10 to 15 minutes.
    [43] [43] After a melt blend of the polymer with the composite is formed, the blend is molded and then cooled to obtain the antibacterial and antistatic polymer material. In this step, any suitable molding apparatus known in the art may be used. In an embodiment, an injection molding machine may be used, and the blend may be injected into a mold in the injection molding machine and then molded by using a tablet machine through hot pressing. The injection head of the injection molding machine may be heated to 60 to 300 °C, and the mold may be heated to 10 to 35 °C. The blend inside the mold may be hot-pressed with upper and lower plates of the tablet machine at 60 to 300 °C and 4 to 10 MPa for 2 to 10 minutes. The blend may be molded into any shape as desired.
    [44] [44] The blend, after being molded, may be cooled to room temperature, preferably to a temperature of 20 to 25 °C, in any known manner.
    [45] [45] A fifth aspect of the present disclosure provides use of the antibacterial and antistatic polymer material in medical device. This is because the polymer material according to the present disclosure has a high antibacterial activity and an excellent antistatic property.
    [46] [46] Various aspects of the present disclosure will now be described in more detail with reference to the following examples, which however should not be construed as limiting the scope of the disclosure.
    [47] [47] Preparation of MWCNTS/Ag heterojunction composite
    [48] [48] Example 1
    [49] [49] 1 g of silver nitrate and 100 ml of a 0.04 mol/L polyethylene glycol (Mw=4000) aqueous solution were mixed and stirred at a stirring speed of 200 rpm for 15 min to form a silver salt solution.
    [50] [50] The silver salt solution was mixed with 3 g of multi-walled carbon nanotubes (having an outer diameter of 5 to 15 nm and a length of 10 to 20 um) in the dark with stirring at a stirring speed of 200 rpm for 1 h to form a suspension.
    [51] [51] The suspension was subjected to ultraviolet irradiation emitted by an ultraviolet irradiation source with a wavelength of 254 nm and power of 25 W to conduct a reduction reaction at 50 °C for 4 h. After completion of the reduction reaction, the resulting product was suction filtered. The residue resulting from the filtration was washed with water (3 times) and then with ethanol (3 times), and was then dried in an oven at 70 °C for 11 h to obtain a MWCNTs@Ag heterojunction composite.
    [52] [52] The obtained composite was subsequently optically examined under a transmission electron microscope (TEM). The TEM image of this composite is shown in FIG. 1. As is clear from this figure, nano silver particles have been uniformly deposited on surfaces of the carbon nanotubes, and no aggregation of the nano silver particles 1s observed.
    [53] [53] Preparation of antibacterial and antistatic polymer material
    [54] [54] Example 2
    [55] [55] A polypropylene (PP) soild was dried at 80 °C for 6 h to obtain 99 g of a dried PP solid. 2 g of liquid paraffin was dripped onto surfaces of the dried PP solid.
    [56] [56] The composite obtained in Example 1 was dried at 90 °C for 6 h.
    [57] [57] The dried PP solid having paraffin thereon was then mixed with 1 g of the dried composite with stirring at a stirring speed of 60 rpm for 5 min to form a mixture.
    [58] [58] The mixture was treated for 10 min using a two-roll mill at 165 °C to give a melt blend. A rotation speed ratio of the front roller to the rear roller of the two-roll mill was controlled at 1:1.35, and the front roller was rotated at a speed of 20 rpm. Thereafter, the melt blend was injected into a mold (at 35 °C) in an injection molding machine with its injection head heated to 200 °C, and was then hot-pressed at 200 °C and 10 MPa for 10 min, After cooling to 25 °C, an antibacterial and antistatic polymer material was obtained in sheet form.
    [59] [59] Example 3
    [60] [60] An antibacterial and antistatic polymer material was prepared as in Example 2, except that the mass of the dried PP was 98.5 g, and the mass of the dried composite was 15g
    [61] [61] Example 4
    [62] [62] An antibacterial and antistatic polymer material was prepared as in Example 2, except that the mass of the dried PP was 98 g, and the mass of the dried composite was
    [63] [63] Example 5
    [64] [64] An antibacterial and antistatic polymer material was prepared as in Example 2, except that the mass of the dried PP was 97.5 g, and the mass of the dried composite was 25g.
    [65] [65] Example 6
    [66] [66] An antibacterial and antistatic polymer material was prepared as in Example 2, except that the mass of the dried PP was 97 g, and the mass of the dried composite was
    [68] [68] APP solid was dried at 80 °C for 6 h.
    [69] [69] 100 g of the dried PP solid was treated for 10 min using a two-roll mill at 165 °C. A rotation speed ratio of the front roller to the rear roller of the two-roll mill was controlled at 1:1.35, and the front roller was rotated at a speed of 20 rpm. Thereafter, the PP was injected into a mold (at 35 °C) in an injection molding machine with its injection head heated to 200 °C, and was then hot-pressed at 200 °C and 10 MPa for 10 min. After cooling to 25 °C, a polymer material was obtained in sheet form.
    [70] [70] Comparative Example 2
    [71] [71] APP solid was dried at 80 °C for 6 h to obtain 99 g of a dried PP solid. 2 g of liquid paraffin was dripped onto surfaces of the dried PP solid.
    [72] [72] Carbon nanotubes were dried at 90 °C for 6 h.
    [73] [73] The dried PP solid having paraffin thereon was then mixed with 1 g of the dried carbon nanotubes with stirring at a stirring speed of 60 rpm for 5 min to form a mixture.
    [74] [74] The mixture was treated for 10 min using a two-roll mill at 165 °C to give a melt blend. A rotation speed ratio of the front roller to the rear roller of the two-roll mill was controlled at 1:1.35, and the front roller was rotated at a speed of 20 rpm. Thereafter, the melt blend was injected into a mold (at 35 °C) in an injection molding machine with its injection head heated to 200 °C, and was then hot-pressed at 200 °C and 10 MPa for 10 min. After cooling to 25 °C, a polymer material was obtained in sheet form.
    [75] [75] Comparative Example 3
    [76] [76] A polymer material was prepared as in Comparative Example 2, except that the mass of the dried PP was 98.5 g, and the mass of the dried carbon nanotubes was 1.5 g.
    [77] [77] Comparative Example 4
    [78] [78] A polymer material was prepared as in Comparative Example 2, except that the mass of the dried PP was 97.5 g, and the mass of the dried carbon nanotubes was 2.5 g.
    [79] [79] Comparative Example 5
    [80] [80] A polymer material was prepared as in Comparative Example 2, except that the mass of the dried PP was 97 g, and the mass of the dried carbon nanotubes was 3 g.
    [81] [81] The antibacterial and antistatic polymer materials prepared in Examples 2 to 6 and the polymer materials prepared in Comparative Examples | to 5 were measured for mechanical properties, conductivity, and antibacterial activity. The results are shown in Table 1.
    [82] [82] It canbe seen from Table 1 that the antibacterial and antistatic polymer materials had better mechanical properties, conductivity, and antibacterial activity.
    [83] [83] The present disclosure has been described with reference to specific embodiments. However, it is clear that the described embodiments are only a part, but not all, of the embodiments of the disclosure. Other embodiments can be conceived by those skilled in the art based on the described embodiments, and shall fall within the scope of the disclosure as defined by the appended claims.
    权利要求:
    Claims (10)
    [1]
    1. MWCNTs/Ag heterojunction composite, comprising carbon nanotubes and nanosilver particles deposited on surfaces of the carbon nanotubes.
    [2]
    The composite of claim 1, wherein the nanosilver particles have a particle size of 3-15 nm.
    [3]
    The composite of claim 1 or 2, wherein a mass ratio of the nanosilver particles to the carbon nanotubes is within a range of 0.19 - 0.23.
    [4]
    A method for making the MWCNTs/Ag heterojunction composite according to any one of claims | — 3, comprising the steps of: mixing a soluble silver salt, the carbon nanotubes and an aqueous solution of polyethylene glycol to form a slurry; and subjecting the suspension to ultraviolet radiation to perform a reduction reaction to obtain the MWCNTs/Ag heterojunction composite.
    [5]
    The method of claim 4, wherein the soluble silver salt is silver nitrate; and wherein a mass ratio of the soluble silver salt to the carbon nanotubes is within a range of (0.5-5):(1-20).
    [6]
    The method of claim 4, wherein the aqueous solution of polyethylene glycol has a molar concentration of 0.04 - 0.08 mol/L; and wherein a mass ratio of the soluble silver salt to volume of the aqueous solution of polyethylene glycol is within a range of (0.5 - 5) g: (50 - 500) ml.
    [7]
    The method of claim 4, wherein the ultraviolet radiation is emitted from an ultraviolet radiation source having a wavelength of 100-365 nm and power of 15-25 W; and wherein the reduction reaction is carried out at a temperature of 30-80°C for 4-8 hours.
    -12-
    [8]
    An antibacterial and antistatic polymeric material comprising a polymer and the MWCTNs/Ag heterojunction composite according to any one of claims 1 to 3 or wherein the MWCNTs/Ag heterojunction composite is made by the method according to any one of claims 4 to 7.
    [9]
    The polymeric material of claim 8, wherein the polymer is polypropylene, polyethylene or polylactic acid; and wherein the polymer is 97-99% by mass with respect to the total mass of the antibacterial and antistatic polymeric material.
    [10]
    A method of making the antibacterial and antistatic polymeric material of claim 8 or 9, comprising the steps of: subjecting the polymer and the MWCNT s/Ag heterojunction composite to melt blending so as to form a melt blend thereof; and subjecting the melt mixture to molding and cooling to obtain the antibacterial and antistatic polymer material.
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    同族专利:
    公开号 | 公开日
    CN112980050A|2021-06-18|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    WO2012177223A1|2011-06-24|2012-12-27|Nanyang Technological University|A nanocomposite, a filtration membrane comprising the nanocomposite, and methods to form the nanocomposite and the filtration membrane|
    AU2020103516A4|2020-03-18|2021-01-28|Ningxia University|Antistatic, antibacterial, and multifunctional polymer composite material, and preparation method thereof|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    CN202110468315.9A|CN112980050A|2021-04-28|2021-04-28|Heterojunction composite material and preparation method thereof, antibacterial and antistatic high polymer material and preparation method and application thereof|
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